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Star-branched ternary integrated rubber prepared through catalysis of mono-scandium-cyclopentadienyl rare earth catalyst and preparation method of star-branched ternary integrated rubber

A rare earth catalyst and branched ternary technology, which is applied in the synthesis of functionalized integrated rubber materials, can solve the problems of poor compatibility, high energy consumption, rubber matrix and filler, etc., and achieve easy synthesis, stable valence state, and simple structure Effect

Active Publication Date: 2022-03-18
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the traditional integrated rubber SIBR lacks polar groups, and the compatibility between the rubber matrix and fillers is poor during processing, requiring a large amount of energy to disperse the rubber matrix and fillers evenly.

Method used

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  • Star-branched ternary integrated rubber prepared through catalysis of mono-scandium-cyclopentadienyl rare earth catalyst and preparation method of star-branched ternary integrated rubber
  • Star-branched ternary integrated rubber prepared through catalysis of mono-scandium-cyclopentadienyl rare earth catalyst and preparation method of star-branched ternary integrated rubber
  • Star-branched ternary integrated rubber prepared through catalysis of mono-scandium-cyclopentadienyl rare earth catalyst and preparation method of star-branched ternary integrated rubber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Example 1 Preparation of macromonomer core A1 containing multiple dangling double bonds (A:B=1, branching agent monomer concentration 3.8g / 100ml, [Si] / [Sc] is 20)

[0048] In a glove box under nitrogen protection, a magnetic stir bar was placed in a 100mL round-bottomed flask, and 30.6mg (60μmol) of scandium monocene rare earth catalyst (C 5 Me 4 SiMe 3 )Sc(CH 2 C 6 h 4 NMe 2 -o) 2 , then add 55.5mg (60μmol) [Ph 3 C][B(C 6 f 5 ) 4 ], add 2mL of toluene solvent under stirring, add 0.230g (1.2mmol) dimethyl dipentadienyl silane under vigorous stirring, react at room temperature for 3min, the molar ratio of dimethyl dipentadienyl silane and rare earth catalyst [Si ] / [Sc] is 20. After the polymerization is complete, take the round bottom flask out of the glove box, add a small amount of methanol to terminate the reaction, then pour a large amount of methanol into the terminated reaction solution, wash the precipitated polymer with methanol, and dry it in a vacuum...

Embodiment 2

[0049] Example 2 Preparation of macromonomer core A2 containing multiple dangling double bonds (A:B=1, branching agent monomer concentration 3.8g / 100ml, [Si] / [Sc] is 20)

[0050] The reaction was carried out at room temperature for 10 minutes, and other polymerization conditions were the same as in Example 1 to obtain a macromonomer core A2 containing multiple pendant double bonds. Polymer structure analysis result is as follows: productive rate is 90% (mass percentage), molecular weight M w 14.3×10 3 g / mol, molecular weight distribution index M w / M n is 3.97, the structure content of the pendant double bond is 41% (mole percent), and the gel content is 10% (mass percent).

Embodiment 3

[0051] Example 3 Preparation of macromonomer core B1 containing multiple dangling double bonds (A:B=1, branching agent monomer concentration 3.8g / 100ml, [Si] / [Sc] is 20)

[0052] In the 100mL round-bottomed flask, a magnetic stirring bar was put into it, and 30.6mg (60 μmol) of a monocene scandium rare-earth catalyst (C 5 h 5 )Sc(CH 2 C 6 h 4 NMe 2 -o) 2 , reacted at room temperature for 10 min, and other polymerization conditions were the same as in Example 1 to obtain a macromonomer core B1 containing multiple pendant double bonds. Polymer structure analysis result is as follows: productive rate is 30% (mass percentage), molecular weight M w 5.0×10 3 g / mol, molecular weight distribution index M w / M n is 1.31, the structure content of the pendant double bond is 87% (mole percent), and the gel content is 0.

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Abstract

The invention belongs to the technical field of functional high polymer materials, and provides star-branched ternary integrated rubber prepared through catalysis of a mono-scandium-cyclopentadienyl rare earth catalyst and a preparation method of the star-branched ternary integrated rubber. The star-branched ternary integrated rubber is prepared by copolymerizing a macromonomer containing a plurality of overhanging double bonds, amino-containing styrene, isoprene and butadiene under the catalysis of a mono-scandium-cyclopentadienyl rare earth catalyst. The content of amino-containing styrene is 5%-50% by mole, and the content of isoprene is 20%-90% by mole; the content of the 3, 4-polyisoprene is 3%-78% based on the total molar amount of the polyisoprene being 100%; the content of the 1, 4-polybutadiene is 50%-98% based on 100% of the total mole of the polybutadiene; the amino-containing styrene is selected from styrene derivatives containing nitrogen substituent groups. The prepared star-branched terpolymer can effectively improve the blending performance of the star-branched terpolymer and a polar filler, increase the acting force between a rubber matrix and the filler, and improve the physical and mechanical properties of a rubber material.

Description

technical field [0001] The invention belongs to the technical field of synthesizing functionalized integrated rubber materials, and in particular relates to the preparation of star-shaped branched ternary integrated rubber catalyzed by a single scandium-cene rare earth catalyst and a preparation method thereof. Background technique [0002] Mono-scandocene rare-earth catalysts have high monomer microstructure stereoselectivity for the polymerization of conjugated olefins (such as monomer styrene, isoprene, and butadiene). Binary or terpolymers of conjugated olefins belong to rare earth rubber materials. This kind of rare earth rubber materials is a kind of synthetic rubber materials with excellent performance, but the preparation of rare earth rubber materials in the prior art is mostly limited to the preparation of Linear rare earth rubber material. Compared with linear rare-earth rubber materials, star-shaped rare-earth rubber materials have the ability to obtain high-mol...

Claims

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Application Information

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IPC IPC(8): C08F275/00C08F236/10C08F212/14C08F4/52
CPCC08F275/00C08F4/52C08F236/10C08F212/28Y02T10/86
Inventor 李杨余佳临牛慧冷雪菲穆晓春王艳色韩丽
Owner DALIAN UNIV OF TECH
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