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Catalyst for synthesizing high trans-1,4 polybutadiene-isoprene rubber material and catalytic synthesis method thereof

A technology of isoprene rubber and polybutadiene, which is applied in the field of high trans-butadiene rubber material synthesis

Active Publication Date: 2021-09-14
JINING UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, at present, there are very few research reports on the application and development of Ti-type Ziegler-Natta catalytic systems containing external electron donors in the trans-1,4 polymerization of conjugated dienes. Therefore, the research and preparation of this type of catalytic system applications It is of great significance for the development of high-performance trans-1,4 rubber new materials

Method used

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  • Catalyst for synthesizing high trans-1,4 polybutadiene-isoprene rubber material and catalytic synthesis method thereof
  • Catalyst for synthesizing high trans-1,4 polybutadiene-isoprene rubber material and catalytic synthesis method thereof
  • Catalyst for synthesizing high trans-1,4 polybutadiene-isoprene rubber material and catalytic synthesis method thereof

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preparation example Construction

[0032] The preparation method of described main catalyst comprises the steps:

[0033] (1) Under an inert gas atmosphere, add a magnesium compound into the ball mill jar, and ball mill at room temperature for 10-48 hours;

[0034] (2) Under an inert gas atmosphere, add titanium halide to the ball milling tank in step (1), and continue ball milling at room temperature for 10-48 hours to obtain a mixture;

[0035] (3) washing the mixture in step (2) with an organic solvent for 2 to 5 times, suction filtering, and drying to obtain a powdery main catalyst;

[0036] Wherein: the mass ratio of the magnesium compound to the titanium halide is 1:0.005-0.200.

[0037] The organic solvent is one or two of anhydrous n-hexane, anhydrous n-heptane, anhydrous cyclohexane, anhydrous toluene, anhydrous chloroform and anhydrous xylene.

[0038] A method for catalyst-catalyzed synthesis of high trans-1,4 polybutadiene-isoprene rubber materials, comprising the following steps: after the reacto...

Embodiment 1～ Embodiment 6 and comparative example I～II

[0042] Preparation of the main catalyst: Vacuumize the ball mill tank, replace with nitrogen, pump and replace three times in sequence, add 14.25g (0.15mol) of anhydrous magnesium chloride carrier under nitrogen atmosphere, grind at room temperature for 12h; add 50mL of anhydrous n-heptane / 0.87mL The mixed solution of titanium tetrachloride was ground again at room temperature for 12 hours, and the catalyst was washed twice with a large amount of anhydrous n-heptane, filtered, and vacuum-dried to obtain a powdery main catalyst, which was analyzed by an ultraviolet spectrophotometer, and the Ti content of the main catalyst was It is 1.74wt.%.

[0043] Polymerization: Vacuumize the 100mL round-bottomed flask (containing magnets), replace with nitrogen, pump and replace three times in sequence, add 42.54g of butadiene / isoprene mixed monomer (0.63mol, monomer and The main catalyst molar ratio is 1:9×10 -5 , the molar ratio of butadiene to isoprene is 1:65.7), 1.71×10 -3 mol trii...

Embodiment 7～ Embodiment 8

[0053] The preparation method of the main catalyst is the same as in Example 1, and the polymerization reaction uses the same reagents and reaction steps as in Example 1, except that the amount of reagents used and the reaction parameters in Table 2 below are different.

[0054] Table 2. Raw material addition amount and reaction parameters

[0055]

[0056]

[0057] Comparing Example 7 with Examples 1, 3, and 5, it can be seen that the catalysts of Example 7 of the present invention and Examples 1, 3, and 5 are all made up of a main catalyst, a cocatalyst and an external electron donor, and the external electron donor is two Phenyldimethoxysilane, but embodiment 7 uses a low reaction temperature of 10°C, a low amount of promoter, a low amount of electron donating, and a low ratio of main catalyst to monomer. Example 7 is a 120min polymerization product, characterized by proton nuclear magnetic resonance spectrometer and gel permeation chromatography, it can be seen that:...

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Abstract

The invention relates to the technical field of synthesis of high-trans-1,4-polybutadiene-isoprene rubber materials, in particular to a catalyst for synthesizing a high-trans-1,4-polybutadiene-isoprene rubber material and a catalytic synthesis method of the catalyst. The catalyst comprises a main catalyst, a cocatalyst and a third component, wherein the third component is an alkoxy silane external electron donor. The method comprises the following steps: pumping, discharging and replacing a reactor, sequentially adding a butadiene / isoprene mixed monomer, a cocatalyst, a third component and a main catalyst / organic solvent mixture to form an active center to initiate monomer polymerization, and conducting reacting at 10-50 DEG C for 1-120 minutes to obtain the trans-1,4-polybutadiene-isoprene rubber material. The external electron donor is introduced into the catalyst, the charging sequence of the monomer, the cocatalyst, the electron donor and the main catalyst is adopted during polymerization, the external electron donor can effectively activate an active center, an active center with higher trans-1,4 steric selectivity is formed, and the steric selectivity of the catalyst is improved.

Description

technical field [0001] The invention relates to the technical field of synthesis of high trans-butadiene rubber materials, in particular to a catalyst for synthesizing high trans-1,4 polybutadiene-isoprene rubber materials and a catalytic synthesis method thereof. Background technique [0002] High trans-1,4 polybutadiene-isoprene rubber material has excellent dynamic properties (such as low rolling resistance, low compression heat generation) and good flex resistance, and is a new type of high-performance Potential material for green tires. The synthesis of high trans-1,4 polydiene rubber materials requires catalysts with high trans-1,4 stereoselectivity and corresponding polymerization processes. [0003] In the field of trans-1,4 rubber synthesis, commonly used catalysts mainly include Ziegler-Natta catalysts such as titanium (Ti) series, vanadium (V) series, chromium (Cr) series, nickel (Ni) series, and rare earth series, among which, Supported Ti-type Ziegler-Natta ca...

Claims

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Application Information

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IPC IPC(8): C08F236/08C08F236/06C08F4/646C08F4/654
CPCC08F236/08C08F236/06C08F4/6465C08F4/6543
Inventor 牛庆涛贺爱华靳满满
Owner JINING UNIV
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