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Hydroxy functionalized polyethylene and preparation method thereof

A technology of hydroxyl polybutadiene and hydroxyl terminated polybutadiene is applied in the field of hydroxyl functionalized polyethylene and its preparation, and can solve the problems of high application cost, difficult recovery, expensive catalyst and the like

Active Publication Date: 2016-06-01
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although ring-opening metathesis polymerization can better realize the functionalization of polar groups, its polymerized monomers are usually cycloolefins, and the yield is not as large as that of traditional olefin monomers; the catalyst is Grubbs catalyst, which is relatively expensive and difficult to recycle, so the application cost higher
In addition, the above method can prepare single-end or double-end hydroxyl functionalized polyethylene, but the preparation of polyhydroxyl functionalized polyethylene has not been reported.

Method used

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  • Hydroxy functionalized polyethylene and preparation method thereof
  • Hydroxy functionalized polyethylene and preparation method thereof

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preparation example Construction

[0031] The preparation method of described polyhydroxy polybutadiene is:

[0032] 1) butadiene rubber epoxidation reaction prepares epoxidized butadiene rubber;

[0033]Mass concentration is 10g / L-100g / L butadiene rubber and epoxidation reagent epoxidation reaction in reaction medium to prepare epoxidized butadiene rubber;

[0034] The molar ratio of the epoxidation reagent to the butadiene structural unit in the butadiene rubber is 1%-40%; the reaction temperature is between 0°C and 80°C; the reaction time is 30 minutes to 12 between hours;

[0035] 2) Oxidative cracking reaction of epoxidized butadiene rubber to prepare polybutadiene liquid rubber with high cis-1,4 content and epoxidized terminal aldehyde group;

[0036] Epoxidized butadiene rubber is reacted in the reaction medium under the action of oxidative cracking reagent to obtain high cis-1,4 content epoxidized terminal aldehyde polybutadiene liquid rubber;

[0037] The concentration of the epoxidized butadiene ru...

Embodiment 1

[0058] Preparation of high cis-terminated hydroxyl polybutadiene :

[0059] Take 5.00g of nickel-based butadiene rubber (BR9000), dissolve it completely in 100mL of tetrahydrofuran, the rubber concentration is 50g / L, keep the temperature at 30°C, add m-chloroperoxybenzoic acid under vigorous stirring, the amount of m-chloroperoxybenzoic acid is The butadiene structural unit in the nickel-based butadiene rubber (BR9000) is 6%, the reaction time is 6 hours, and the product is precipitated with a large amount of ethanol and vacuum-dried. product by 1 HNMR showed that the epoxy rate was 6%.

[0060] Take 4.00g of the above-mentioned epoxidized butadiene rubber, completely dissolve it in 100mL of tetrahydrofuran, the rubber concentration is 40g / L, keep the temperature at 30°C, add periodic acid under vigorous stirring, the molar ratio of periodic acid to epoxy group is 1 : 1, reacted for 30 minutes. The product can be filtered to obtain polybutadiene liquid rubber with high ci...

Embodiment 2

[0065] The preparation process of high cis-terminated hydroxyl polybutadiene is the same as in Example 1

[0066] Take 2.0 g of high cis-hydroxyl-terminated polybutadiene, with a cis-1,4 content of 95%, a hydroxyl functionality of 2.0, a number average molecular weight of 5000 g / mol, and a molecular weight distribution of 1.6. Add 50mL of cyclohexane, transfer the high cis-hydroxyl-terminated polybutadiene solution into the pressure reactor, add nickel naphthenate-triisobutylaluminum, keep the argon atmosphere, heat to 50°C, and pass in hydrogen, Keep the pressure at 0.5 MPa and react for 4 hours. After the reaction is finished, the telechelic hydroxyl-functionalized polyethylene is obtained through cooling, precipitation, separation, purification and drying.

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Abstract

The invention discloses a hydroxy functionalized polyethylene and a preparation method thereof. The hydroxy functionalized polyethylene is characterized by comprising telechelic hydroxy polyethylene and polyhydroxy polyethylene; the polyhydroxy polyethylene is characterized in that hydroxyls are positioned at head and tail ends of a polyethylene molecular chain and in the molecular chain. The method includes: (1) hydrogenating high-cis-1,4-hydroxyl-terminated polybutadiene to prepare telechelic hydroxy functionalized polyethylene; (2) hydrogenating polyhydroxy polybutadiene liquid rubber to prepare polyhydroxy polyethylene. The hydroxy functionalized polyethylene is rich in raw material source and adjustable in position and quantity of hydroxyls, the preparation method is simple, convenient and efficient, and structural clearness, excellent performances and extensive application prospect are realized.

Description

technical field [0001] The invention relates to a hydroxyl-functionalized polyethylene and a preparation method thereof. The hydroxyl-functionalized polyethylene is prepared by hydrogenating high-cis-type hydroxyl-terminated polybutadiene or polyhydroxypolybutadiene, including telechelic-type hydroxylated polyethylene. and polyhydroxypolyethylene. The hydroxyl-functionalized polyethylene has rich sources of raw materials, adjustable hydroxyl position and quantity, simple and efficient preparation method, clear structure and excellent performance, and has broad application prospects in the field of new materials. Background technique [0002] Polyolefin plastics, that is, polymers of olefins, are the polymer materials with the largest output and the most applications, among which polyethylene and polypropylene are the most important. Due to the characteristics of abundant raw materials, low price, easy processing and molding, and excellent comprehensive performance, it is wi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08C19/02C08C19/08C08C19/06C08C19/00C08F136/06C08F8/04
CPCC08C19/00C08C19/02C08C19/06C08C19/08C08F8/04C08F136/06
Inventor 介素云李伯耿周勤灼
Owner ZHEJIANG UNIV
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