Preparation method of copolymer of olefin and unsaturated carboxylic acid

An unsaturated, copolymer technology, applied in the field of polymer preparation, can solve the problems of expensive equipment, high temperature and high pressure conditions, and high energy consumption, and achieve the effect of improving the effect of balling

Pending 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

Although high-pressure free radical copolymerization can directly introduce polar monomers into polyolefin chains, this method requires high temperature and high pressure conditions, high energy consumption, and expensive equipment

Method used

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  • Preparation method of copolymer of olefin and unsaturated carboxylic acid
  • Preparation method of copolymer of olefin and unsaturated carboxylic acid
  • Preparation method of copolymer of olefin and unsaturated carboxylic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0111] 1) Ligand L 1 Preparation of:

[0112] The preparation of complex (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 is ethyl, M is nickel, Y is O, X is Br)

[0113] 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 ...

Embodiment 2

[0119] 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 8.0 mg (5 μmol) of the complex Ni 1 , 50mL dichloromethane, 30mmol (5.10g) 2,2-dimethyl-7-octenoic acid, 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.

Embodiment 3

[0121] 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 8.0 mg (5 μmol) of the complex Ni 1 , 100mL dichloromethane, 30mmol (5.10g) 2,2-dimethyl-7-octenoic acid, 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.

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Abstract

The invention relates to a preparation method of a copolymer of olefin and unsaturated carboxylic acid and the copolymer prepared by the method. The method comprises the step of polymerizing olefin and unsaturated carboxylic acid in the presence of a catalyst, an improver, an optional chain transfer agent and an improver, wherein the used catalyst 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 by the preparation method has a good prospect in industrial application.

Description

technical field [0001] The invention belongs to the field of polymer preparation, in particular to a method for preparing a copolymer of olefin and unsaturated carboxylic acid. Background technique [0002] Polyolefin products are low in price, excellent in performance and wide in application. Under the condition of retaining the excellent physical and chemical properties of the original 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 , endowing it with new properties that its raw materials do not have. Although high-pressure radical copolymerization can directly introduce polar monomers into polyolefin chains, this method requires high temperature and high pressure conditions, high energy consumption, and expensive equipment. [0003] Coordination catalytic copolymerization, as a normal temperature and p...

Claims

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Application Information

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IPC IPC(8): C08F210/02C08F220/64C08F4/70
CPCC08F210/02C08F2410/03C08F220/64C08F2500/24C08F4/7006
Inventor 高榕郭子芳张晓帆周俊领赖菁菁李昕阳刘东兵顾元宁安京燕
Owner CHINA PETROLEUM & CHEM CORP
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