Preparation method of ethylene-styrene derivative copolymer

A technology of styrene derivatives and copolymers, applied in the field of preparation of ethylene-styrene derivatives copolymers

Active Publication Date: 2018-09-14
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, there is no rare earth catalyst system that can catalyze the random copolymerization of ethylene and styrene to prepare ethylene-styrene quasi-random copolymers (that is, there are no continuous styrene structural units in the copolymer)

Method used

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  • Preparation method of ethylene-styrene derivative copolymer
  • Preparation method of ethylene-styrene derivative copolymer
  • Preparation method of ethylene-styrene derivative copolymer

Examples

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preparation example Construction

[0036] A kind of preparation method of ethylene-styrene derivative copolymer provided by the invention, concrete steps are as follows:

[0037] a) under the protection of an inert gas such as nitrogen or argon, dissolving the rare earth catalyst composition in an organic solvent to obtain a rare earth catalyst composition solution;

[0038] b) using ethylene and styrene derivative monomers as raw materials, using the rare earth catalyst composition solution to catalyze the polymerization reaction, sedimenting the product, and drying to obtain an ethylene-styrene derivative copolymer;

[0039] Polymerization The solution polymerization is carried out in the presence of a solvent. The organic solvent is selected from one or a mixture of saturated alkanes, aromatic hydrocarbons, halogenated aromatic hydrocarbons and cycloalkanes. Preferred is one or a mixture of n-hexane, n-heptane, petroleum ether, cyclohexane, benzene, ethylbenzene, toluene, xylene, chlorobenzene, dichlorobenz...

Embodiment 12

[0104] Example 12: Under anhydrous and oxygen-free conditions, the rare earth complex 1 (6.0 mg, 10 μmol) and [Ph 3 C][B(C 6 f 5 ) 4 ] (9.2mg, 10μmol) of toluene solution 5mL, at 70 ° C, was added to 100mL filled with styrene (4.16g, 40mmol) monomer and Ai i Bu 3 (0.4mL×0.5M) in ethylene-saturated toluene (25mL). Then keep the ethylene pressure constant and react for 1 hour, add a small amount of ethanol solution to terminate the polymerization reaction. Then the reaction solution was poured into 100 mL ethanol containing a small amount of hydrochloric acid and stabilizer (BHT) for sedimentation. The obtained polymer was dried in a vacuum oven at 50° C. for 48 hours to obtain a polymer with a net weight of 1.26 g.

Embodiment 1～47

[0105] Examples 1-47: The experimental procedure of this series of examples is the same as that of Example 12, and the polymerization reaction conditions and the change conditions of the catalytic system are described in Table 1 in detail.

[0106] Table 1 Composition of Rare Earth Complex 1 Catalyzes Copolymerization of Ethylene and Styrene

[0107]

[0108]

[0109] Table 2 Different types of rare earth complex composition composition catalyzed copolymerization of ethylene and styrene derivatives

[0110]

[0111] Note: a p-methylstyrene, b p-fluorostyrene; A is [Ph 3 C][B(C 6 f 5 ) 4 ], B is [PhNMe 2 H][B(C 6 f 5 ) 4 ], C is [NEt 3 H][B(C 6 f 5 ) 4 ].

[0112] Carry out carbon nuclear magnetic resonance spectrum analysis to above-mentioned ethylene-styrene derivative copolymer, as Figure 1~3 shown. Depend on figure 1 It can be seen that the ethylene-styrene copolymer chain microstructure prepared in Example 9 does not contain styrene continuous struct...

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Abstract

The invention relates to a preparation method of an ethylene-styrene derivative copolymer and belongs to the technical field of high polymer materials. The preparation method of the ethylene-styrene derivative copolymer, provided by the invention, has the benefits that the copolymerization of an ethylene and styrene monomer is catalyzed by utilizing a restricted geometrically-configured rare earthcatalyst composition for the first time, so that the ethylene-styrene derivative quasi-random copolymer is prepared. The copolymer only can be prepared by a restricted geometrically-configured titanium catalyst system previously. Therefore, the preparation method of the ethylene-styrene derivative quasi-random copolymer is very innovative, and a new technical route for the preparation of the ethylene-styrene derivative quasi-random copolymer is developed.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a preparation method of an ethylene-styrene derivative copolymer. Background technique [0002] Ethylene, styrene and its derivatives are two types of monomers with very different properties, and it is impossible to use free radical polymerization method and traditional Ziegler-Natta catalytic system to carry out copolymerization to prepare ethylene-styrene monomer copolymers. The invention of the single-active catalytic system makes the copolymerization of these two types of monomers possible. To this end, people have invested a lot of energy to develop a series of catalytic systems for the copolymerization of ethylene-styrene monomers. Among them, when the single-site, homogeneous group IV metal catalyst system catalyzes the copolymerization of ethylene and styrene monomers, there is a problem of low insertion rate of styrene monomers. During the copolym...

Claims

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Application Information

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IPC IPC(8): C08F210/02C08F212/08C08F212/12C08F212/14C08F4/52
CPCC08F210/02C08F4/52C08F212/08C08F2500/03C08F212/12C08F212/14
Inventor 李世辉崔冬梅
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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