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Method for preparing olefin-olefin alcohol copolymer

A technology of olefin alcohols and copolymers, which is applied in the field of high molecular polymer preparation, can solve the problems of polymer transport solvent removal, difficult granulation, scaling, etc., and achieve the effects of convenient transportation, not easy to scale, and simple preparation process

Active Publication Date: 2021-05-04
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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  • Method for preparing olefin-olefin alcohol copolymer
  • Method for preparing olefin-olefin alcohol copolymer
  • Method for preparing olefin-olefin alcohol copolymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0117] 1) Ligand L 1 Preparation of:

[0118] Under the protection of nitrogen, 2,6-diethylaniline (2.0mL, 12mmol) was dissolved in 20mL of toluene, and 12mL of trimethylaluminum (1.0M, 12mmol) was added dropwise at room temperature, and the reaction was refluxed for 2 hours, and the system was cooled to room temperature. Camphorquinone (0.831g, 5mmol) was added, and the system was refluxed for 6h. The reaction product was neutralized by aqueous sodium hydroxide solution, extracted and dried with dichloromethane, and the yellow ligand L was obtained by column chromatography. 1 , the yield was 69.2%. 1 H-NMR (CDCl 3 ):δ6.94-6.92(m,6H,C Ar -CH 3 ),2.56-2.51(m,4H,C Ar -CH 3 ),2.36-2.31(m,4H,C Ar -CH 3 ),1.82-1.78(m,4H,CH 2 ),1.54(m,1H),1.24-1.18(m,12H),1.09(s,3H,CH 3 ),0.94(m,6H,CH 3 ).

[0119] 2) Complex Ni 1 (R in structural formula III 1 , R 3 is ethyl, R 2 , R 4 -R 7 , R 10 for hydrogen, R 8 , R 9 and R 11 is methyl, R 12 Be ethyl, M is nickel, Y is O...

Embodiment 2

[0124] The present embodiment adopts the prepared catalyst Ni of embodiment 1 1 , the difference from Example 1 is: 2-methyl-2-hydroxyl-7-octene and AlEt 3The consumption is 2 times of embodiment 1.

[0125] 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 8.0 mg (5 μmol) of the complex Ni 1 , 30mmol (5.1mL) 2-methyl-2-hydroxy-7-octene, 30mL 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.

[0126] figure 2 Photographs of spherical and / or quasi-spherical polymers produced in this exa...

Embodiment 3

[0128] The present embodiment adopts the prepared catalyst Ni of embodiment 1 1 , The difference from Example 1 is that the polymerization temperature is 60°C.

[0129] 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 8.0 mg (5 μmol) of the complex Ni 1 , 30mmol (5.1mL) 2-methyl-2-hydroxy-7-octene, 30mL 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 an olefin-olefin alcohol copolymer and an olefin-olefin alcohol copolymer prepared thereby. A catalyst used in the method for preparing the olefin-olefin alcohol copolymer comprises a diimine metal complex as shown in a formula I which is described in the specification. The spherical and / or sphere-like polymer prepared according to a preferred embodiment of the preparation method 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 olefin-olefin alcohol copolymers. 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 intro...

Claims

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Application Information

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IPC IPC(8): C08F210/02C08F216/04C08F4/70C07F15/04
CPCC08F210/02C07F15/045C08F2410/03C08F216/04C08F2500/24C08F4/7006
Inventor 高榕郭子芳刘东兵周俊领李昕阳赖菁菁顾元宁张军辉黄廷杰
Owner CHINA PETROLEUM & CHEM CORP
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