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Preparation method of olefin-olefin alcohol copolymer

A technology for olefin alcohols and copolymers, which is applied in the field of preparation of olefin-olefin alcohol copolymers, can solve the problems of polymer transport solvent removal, difficult granulation, fouling, etc., and achieve good industrial application prospects and good morphology Effect

Active Publication Date: 2020-05-08
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the prior art, no matter what method is used for polymerization, the obtained polymer is a viscous massive solid, which is easy to foul in the polymerization equipment, and brings difficulties to the transportation, solvent removal, and granulation of the polymer.

Method used

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  • Preparation method of olefin-olefin alcohol copolymer
  • Preparation method of olefin-olefin alcohol copolymer
  • Preparation method of olefin-olefin alcohol copolymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0104] 1) Preparation of ligand:

[0105] 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 ).

[0106] 2) Preparation of complex 1: 10ml (DME) NiBr 2 (277mg, 0.9mmol) in dichloromethane solution was added dropwise to 10ml of ligand L1 (350mg, 0.9mmol) in dichloromethane solution, stirred at room temperature for 6 hours, a precipitate precipitated, filtere...

Embodiment 2

[0109] 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 Gas replacement 3 times. Inject 500 mL of hexane into the polymerization system, and simultaneously add 6.1 mg (10 μmol) of complex 1, 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 20°C, keep ethylene pressure of 10atm, and stir for 30min. Finally, it was neutralized with an ethanol solution acidified with 5 volume % hydrochloric acid to obtain a polymer. The polymerization activity and the performance parameters of the polymer are shown in Table 1.

[0110] figure 1 and figure 2 The electron micrographs of the spherical and / or quasi-spherical polymer prepared in this embodiment and after cutting are shown, and it can be seen that the spherical polymer has a cavity inside.

Embodiment 3

[0112] 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 Gas replacement 3 times. Inject 500 mL of hexane into the polymerization system, and simultaneously add 6.1 mg (10 μmol) of complex 1, 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 5 volume % 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 invention discloses a preparation method of an olefin-olefin alcohol copolymer. The method comprises: in the presence of an alkane solvent, carrying out a contact reaction on olefin, olefin alcohol represented by a formula I, a catalyst and an optional chain transfer agent to generate the olefin-olefin alcohol copolymer, wherein in the formula I, L1-L3 are respectively and independently selected from H and C1-C30 alkyl, L4 is C1-C30 alkylene with a side group, and the C1-C30 alkyl is optionally substituted by a substituent. The prepared copolymer is good in form and has a good prospect inindustrial application.

Description

technical field [0001] The invention relates to a preparation method of olefin-olefin alcohol copolymer. 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 radical copolymerization can directly introduce copolymerized polar monomers into polyolefin chains, this ...

Claims

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Application Information

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IPC IPC(8): C08F210/02C08F4/70
CPCC08F210/02C08F4/7006
Inventor 高榕郭子芳周俊领宋文波张晓帆李岩林洁傅捷赖菁菁
Owner CHINA PETROLEUM & CHEM CORP
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