Method for preparing high-vinyl butadiene-styrene copolymer by adopting molybdenum-series catalytic system

A high-vinyl styrene-butadiene copolymer and catalytic system technology, applied in the field of polymer synthesis, can solve the problems of low styrene activity, low styrene polymerization activity, and low styrene content, and achieve low gel content, good Processability, effect of low glue viscosity

Active Publication Date: 2017-05-24
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The activity of the catalytic system to styrene is very low, and the styrene content in the copolymer is less than 2% when the two monomers are fed in an equal molar ratio and the low conversion rate is controlled.
However, the styrene content of the copolymer obtained by the catalytic system is low, and under the condition of equimolar ratio feeding and low conversion rate control, the styrene content in the copolymer is less than 4%.
[0010] Molybdenum-based catalysts are one of the main coordination catalysts for the synthesis of high-vinyl butadiene rubber, but molybdenum-based catalysts have low activity for styrene polymerization and are difficult to apply to the production of high-vinyl styrene-butadiene copolymers
So far, there is no report on the preparation of styrene-butadiene copolymers and styrene-butadiene copolymers with high vinyl structural units using molybdenum (Mo) catalyst systems

Method used

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  • Method for preparing high-vinyl butadiene-styrene copolymer by adopting molybdenum-series catalytic system
  • Method for preparing high-vinyl butadiene-styrene copolymer by adopting molybdenum-series catalytic system
  • Method for preparing high-vinyl butadiene-styrene copolymer by adopting molybdenum-series catalytic system

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Embodiments 1 to 41 are specific implementations of a method for preparing high vinyl styrene-butadiene copolymers using a molybdenum-based catalytic system of the present invention. Wherein embodiment 1 is the best embodiment.

Embodiment 1~6

[0035] This group of examples is a copolymerization reaction of different dosages of TBP ligands.

[0036] A solution prepared by sequentially adding toluene, styrene (St), and butadiene (Bd) into an anhydrous and oxygen-free 20mL reaction flask, the monomer concentration is [M]=3.04×10 -3 mol / mL, W St / W Bd =1 / 3, and then add m-cresol aluminum cocatalyst, main catalyst with different P / Mo ratio and polar additives. Where Al / Mo=5, Mo / Bd=1×10 -3 , dioxane / Mo=0.5. After polymerization at 70°C for 9 hours, terminate the reaction with 1.5-2.0 mL of absolute ethanol, add ethanol to precipitate the copolymer, and dry to remove the solvent.

[0037] Table 1

[0038] .

Embodiment 7~11

[0040] The embodiment of this group is the copolymerization reaction with different dosages of Mo as the main catalyst.

[0041] The experiment was carried out in a sealed nitrogen-protected 20mL polymerization tube, and a solution made of toluene, styrene, and butadiene was added in sequence, and the monomer concentration was [M]=3.04×10 -3 mol / mL, W St / W Bd =1 / 3, then add m-cresol aluminum cocatalyst and polar additive, main catalyst (wherein P / Mo=4), Al / Mo=5, dioxane / Mo=0.5. After polymerization at 70°C for 9 hours, terminate the reaction with 1.5-2.0 mL of absolute ethanol, add ethanol to precipitate the copolymer, and dry to remove the solvent.

[0042] Table 2

[0043] .

[0044] attached by figure 1 The polymer obtained by the GPC test is a unimodal distribution, and the molecular weight of the polymer and its molecular weight distribution are shown in the table below.

[0045] table 3

[0046] .

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Abstract

The invention discloses a method for preparing high-vinyl butadiene-styrene copolymer by adopting a molybdenum-series catalytic system, and belongs to the field of synthesis and research of copolymers. The method comprises the following steps: adding a mixed solution which is prepared by taking styrene and butadiene as monomers, and saturated alkane or / and arene as a solvent, a main catalyst which is obtained by reacting an oxide of molybdenum and / or chloride of molybdenum and a phosphorous-containing compound, a co-catalyst and a polar additive into a nitrogen protected container in sequence; performing coordinate polymerization at 30 to 80 DEG C, terminating, precipitating and drying to obtain the high-vinyl butadiene-styrene copolymer. The co-catalyst is an alkyl magnesium compound or an alkyl aluminium compound; the phosphorous-containing compound is a phosphate compound or a phosphite compound. The high-vinyl butadiene-styrene copolymer prepared with the method is low in gel content and low in adhesive viscosity, and can be used for preparing a modifying agent for high-performance plastics, such as high-performance tire tread rubber, high impact polystyrene and ABS.

Description

technical field [0001] The invention belongs to the field of polymer synthesis research, and in particular relates to a method for preparing a high vinyl styrene-butadiene copolymer by using a molybdenum-based catalyst system. Background technique [0002] The styrene-butadiene copolymer is dominated by styrene-butadiene rubber. Styrene-butadiene rubber is the most widely used synthetic rubber at present. There are mainly two types of emulsion-polymerized styrene-butadiene rubber and solution-polymerized styrene-butadiene rubber. It is a kind of rubber with good comprehensive properties. Mainly used in tire industry, auto parts, rubber hose, tape, rubber shoes, wire and cable and other rubber products. At present, the main methods of synthesizing styrene-butadiene rubber are free radical emulsion polymerization (ESBR) and anionic solution polymerization (SSBR). [0003] Typical ESBR production process: butadiene and styrene are used as the main raw materials, water is the m...

Claims

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Application Information

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IPC IPC(8): C08F236/10C08F4/69
Inventor 华静耿洁婷徐玲肖勇明武祁李迎焦胜成贾凤玲艾学芹庞先明
Owner CHINA PETROLEUM & CHEM CORP
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