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Terminal group-functionalized polyethylene and preparation method thereof

A technology of terminal double-bond polyethylene and polyethylene, which is applied in the field of terminal functionalized polyethylene and its preparation, can solve the problems of limited functionalization research, and achieve the effect of simple and efficient preparation method, clear structure and high yield

Inactive Publication Date: 2014-01-01
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, considerable progress has been made in the research of polyolefins with terminal double bonds, but their further functionalization research is relatively limited.

Method used

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  • Terminal group-functionalized polyethylene and preparation method thereof
  • Terminal group-functionalized polyethylene and preparation method thereof
  • Terminal group-functionalized polyethylene and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] A 500ml dry three-neck flask was pumped three times successively with nitrogen and polymer grade ethylene gas, then filled with ethylene gas and injected with a certain amount of toluene, the iron-based catalyst (toluene solution) and methylaluminoxane (toluene solution), at 30 After reacting at ℃ for 30 minutes, the white solid was collected by filtration, washed with alcohol and deionized water, and dried under vacuum at 50℃ to obtain the initial terminal double-bond polyethylene (defined as "v-PE0").

[0061] The above v-PE0 was extracted with boiling n-hexane for 12 hours, and the solvent was removed to obtain terminal double bond polyethylene (defined as "v-PE1"); Double-bond polyethylene (defined as "v-PE2"; cyclohexane insoluble matter was collected to obtain terminal double-bond polyethylene (defined as "v-PE3".

[0062] 1 H NMR and 13 C NMR characterization confirms that the above-mentioned terminal double-bond polyethylene v-PE (including v-PE0, v-PE1, v-PE2...

Embodiment 2

[0064] In a 250ml two-necked bottle, add 5g of v-PE0 described in Example 1, vacuum dry at 40°C for 1 hour, fill with nitrogen, add 70ml of xylene, heat up to 110°C, stir to fully dissolve. Add 0.5g phosphomolybdenum heteropolyacid X under nitrogen atmosphere 7 PMo 12 o 42 [X=N(CH 3 ) 4 ], 0.12g methyl trioctyl ammonium bisulfate. After stirring evenly, slowly add 5ml of 30wt% hydrogen peroxide dropwise. Continue to stir and react for 5 hours, precipitate the polymer with a large amount of methanol, filter, wash repeatedly with formic acid and dry in vacuum at 50°C for 12 hours to obtain epoxy group-terminated polyethylene, the structure of which is shown in formula (I) (R is structure a).

[0065] 1 H NMR and 13 C NMR characterization confirmed that the polyethylene terminal unsaturated double bonds were completely converted into epoxy groups.

Embodiment 3

[0067] In a 250ml two-necked bottle, add 4g of double-bond-terminated polyethylene v-PE1 described in Example 1, vacuum-dry at 40°C for 1 hour, fill with nitrogen, add 30ml of heptane, heat up to 65°C, and stir to fully dissolve it. Add 2g of m-chloroperbenzoic acid under a nitrogen atmosphere, react for 2 hours, precipitate the polymer with a large amount of methanol, filter, wash with formic acid repeatedly at 50°C and dry in vacuum for 12 hours to obtain epoxy group-terminated polyethylene, the structure of which is shown in formula (I) ( R is shown in structure a).

[0068] 1 H NMR and 13 C NMR characterization confirmed that the polyethylene terminal unsaturated double bonds were completely converted into epoxy groups.

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Abstract

The invention provides terminal group-functionalized polyethylene which is characterized by comprising the following structure as shown in the specification, wherein PE shows a polyethylene chain, and R has a structure shown by a or b; R1 is selected from H, carries or does not carry hetero atoms (such as O, S, P, N, Cl and I) or alkyl of C1-C15 of aryl (such as phenyl). The invention further provides a preparation method of the terminal group-functionalized polyethylene. The terminal group-functionalized polyethylene is abundant in source of active ingredients; the preparation method is simple and convenient and efficient, low in cost, high in product yield, clear in structure, and excellent in performance, and has wide potential application prospects.

Description

technical field [0001] The present invention relates to end group functionalized polyethylene and its preparation method. Background technique [0002] Polyolefin has excellent performance and low price. It is widely used in daily life, industry, agriculture and other fields. It is the largest synthetic resin variety in the world. The molecular structure of general-purpose polyolefin materials is composed of simple saturated hydrocarbon units and lacks polar groups, resulting in poor printing and compatibility of polyolefin materials, which limits its application to a certain extent. Terminal-functionalized polyolefins play an irreplaceable role in the preparation of block / graft and other complex topology polymers; this specific hybrid structure can maintain the original excellent properties of the corresponding constituent units (such as polyolefin units) At the same time, it can significantly improve the compatibility of polyolefins with other materials. Terminal-functio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F8/08C08F110/02C08F4/70C08F8/30C08F8/32C08F8/36C08F8/04C08F8/06
Inventor 李化毅张勇杰胡友良
Owner INST OF CHEM CHINESE ACAD OF SCI
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