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Method for preparing hydroxyl group-containing olefin copolymer and product and application thereof

A technology of olefin copolymer and hydroxyl group, which is applied in the field of polymer polymer preparation, and achieves the effects of improving spheroidizing effect, good appearance and simple preparation process

Active Publication Date: 2021-12-07
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since vinyl alcohol cannot exist independently in the form of monomers, it is usually obtained by free radical polymerization of ethylene-vinyl acetate, and the copolymer undergoes alcoholysis reaction, but a large amount of solvent needs to be used in the alcoholysis process, and the final The saponification product contains a large amount of impurities such as acetic acid and alkali metal salts, and requires a large amount of water for washing

Method used

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  • Method for preparing hydroxyl group-containing olefin copolymer and product and application thereof
  • Method for preparing hydroxyl group-containing olefin copolymer and product and application thereof
  • Method for preparing hydroxyl group-containing olefin copolymer and product and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0134] 1) Preparation of Ligand L1:

[0135]1.5ml 2,6-dimethylaniline (12mmol) was reacted with 57ml 1M trimethylaluminum in toluene, after reflux for 3h, camphorquinone (1.05g, 5mmol) was added, and the reaction was reflux for 8 hours. The reaction was terminated with sodium / ice water, extracted with ethyl acetate, the organic phases were combined, and dried over anhydrous magnesium sulfate. The product was separated by petroleum ether / ethyl acetate column chromatography to obtain a colorless crystal ligand L1 with a yield of 70.2%. 1 HNMRδ(ppm)7.00-6.89(m,6H,Ar-H),3.57(s,1H,NH),2.18(s,6H,CAr-CH 3 ),2.05(s,6H,CH 3 ),1.74(m,4H,CH 2 ),1.44(s,3H,CH 3 ),1.35(m,1H),1.21(s,3H,CH 3 ),1.01(s,3H,CH 3 ),0.87(s,3H,CH 3 ).

[0136] 2) Preparation of complex Ni1: 10ml (DME) NiBr 2 (277mg, 0.9mmol) in ethanol (10mL) was added dropwise to 10ml of ligand L1 (233mg, 0.6mmol) in dichloromethane (10mL), stirred at room temperature for 6 hours, a precipitate precipitated, filtered, washe...

Embodiment 2

[0139] Dry the 1L stainless steel polymerization kettle equipped with mechanical stirring at 130 ° C for 6 hours, vacuumize while it is hot and use N 2 Air replacement 3 times. Inject 500 mL of hexane into the polymerization system, and simultaneously add 7.6 mg (5 μmol) of the complex Ni1, 50 mL of dichloromethane, 30 mmol (5.1 mL) of 2-methyl-2-hydroxy-7-octene, 30 mL of AlEt 3 (1.0mol / L hexane solution), 6.5mL MAO (1.53mol / L toluene solution), at 30°C, keep 10atm ethylene pressure, and stir for 30min. Finally, it was neutralized with an ethanol solution acidified with 10 wt% hydrochloric acid to obtain a polymer. The polymerization activity and the performance parameters of the polymer are shown in Table 1.

Embodiment 3

[0141] Dry the 1L stainless steel polymerization kettle equipped with mechanical stirring at 130 ° C for 6 hours, vacuumize while it is hot and use N 2 Air replacement 3 times. Inject 500 mL of hexane into the polymerization system, and simultaneously add 7.6 mg (5 μmol) of the complex Ni1, 100 mL of dichloromethane, 30 mmol (5.1 mL) of 2-methyl-2-hydroxy-7-octene, 30 mL of AlEt 3 (1.0mol / L hexane solution), 6.5mL MAO (1.53mol / L toluene solution), at 60°C, keep 10atm ethylene pressure, and stir for 30min. Finally, it was neutralized with an ethanol solution acidified with 10 wt% hydrochloric acid to obtain a polymer. The polymerization activity and the performance parameters of the polymer are shown in Table 1.

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Abstract

The present invention relates to a method for preparing a hydroxyl group-containing olefin copolymer and a hydroxyl group-containing olefin copolymer prepared by the method. The method for preparing the hydroxyl group-containing olefin copolymer comprises the step that olefin and olefin alcohol are subjected to polymerization reaction in the presence of a catalyst, an improver and an optional chain transfer agent, wherein the used catalyst comprises a diimine metal complex shown in the formula I in the specification. According to the preparation method, the spherical and / or sphere-like polymer can be prepared and has a good prospect in industrial application.

Description

technical field [0001] The invention belongs to the field of polymer preparation, and in particular relates to a method for preparing a hydroxyl-containing olefin copolymer and its product and application. Background technique [0002] Polyolefin products are low in price, excellent in performance and wide in application. Under the condition of retaining the original excellent physical and chemical properties of polyolefin, introducing polar groups into the polyolefin molecular chain through chemical synthesis can improve its chemical inertness, printing and dyeing properties, wettability and compatibility with other materials properties, endowing it with new properties that its raw materials do not have. At present, most industries use high-pressure free radical polymerization to promote the direct copolymerization of olefins and polar monomers, such as ethylene-vinyl acetate, ethylene-methyl methacrylate, and ethylene-acrylic acid copolymers. Although high-pressure radic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F210/02C08F4/70C08F216/04
CPCC08F210/02C08F2410/03C08F4/7006C08F216/04C08F2500/03C08F2500/24
Inventor 高榕郭子芳周俊领林洁赖菁菁李昕阳顾元宁安京燕
Owner CHINA PETROLEUM & CHEM CORP
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