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Catalyst for polydiene synthesis and preparation method thereof

A polydiene and catalyst technology, which is applied in the field of polydiene synthesis catalyst and its preparation, can solve the problems of unfavorable application, difficult control of catalyst form and catalyst particle size, limited reaction temperature and the like, and achieves low crystallinity, The effect of good fluidity and high trans content

Active Publication Date: 2015-04-22
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the above-mentioned catalysts are prepared by a grinding process, and its catalyst morphology and catalyst particle size are difficult to control
And in the polymerization process, this method uses hydrogenated gasoline as a solvent, so that the reaction temperature is limited, and high temperature polymerization will also affect the morphology, fluidity and catalyst activity of the obtained polymer, which is not conducive to the application

Method used

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  • Catalyst for polydiene synthesis and preparation method thereof
  • Catalyst for polydiene synthesis and preparation method thereof
  • Catalyst for polydiene synthesis and preparation method thereof

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preparation example Construction

[0058] Correspondingly, the application provides a method for preparing a catalyst for polydiene synthesis, comprising the following steps:

[0059] 1) The spherical carrier reacts with the active component, and the main catalyst precursor is obtained after heating up; the spherical carrier is magnesium chloride alcoholate or spherical silica, and the active component is titanium halide, vanadium one or more of halides, titanium oxyhalides and vanadium oxyhalides;

[0060] 2) reacting the procatalyst precursor with a phosphate compound, and continuing to heat up to obtain a procatalyst; the procatalyst includes a spherical carrier, an active component loaded on the spherical carrier, and a phosphate compound;

[0061] 3) The main catalyst and the co-catalyst are added to the polymerization system to catalyze the polymerization of the diene during the synthesis process of the polydiene.

[0062] This application improves the preparation process of the catalyst, uses spherical ...

Embodiment 1

[0079] (1) carrier preparation

[0080] In a 250mL glass reactor equipped with a reflux condenser, a mechanical stirrer and a thermometer, and fully replaced with nitrogen, add 36.5mL of absolute ethanol and 21.3g of anhydrous magnesium chloride (ratio of magnesium alcohol to 2.8:1), and stir After the magnesium chloride is completely dissolved, add 75mL of white oil and 75mL of silicone oil, stir and mix, and maintain at 120°C for 1 hour to obtain a uniformly dispersed emulsion;

[0081] Through the emulsifier, under the condition of pressure of 0.3MPa and emulsifier speed of 3000r / min, the obtained emulsion is sprayed into another stirred reactor containing 1600mL of hexane and cooled to -25°C in advance , keep the temperature of hexane not higher than -10°C, stir for 30 minutes, filter, wash with dry hexane, wash away the silicone oil and white oil, vacuum dry and sieve, and obtain a spherical carrier of 30 μm to 50 μm, its composition MgCl 2 2.38C 2 h 6 O.

[0082] (2...

Embodiment 2

[0088] (1) carrier preparation

[0089] In a 250mL glass reactor equipped with a reflux condenser, a mechanical stirrer and a thermometer, and fully replaced with nitrogen, add 36.5mL of absolute ethanol and 21.3g of anhydrous magnesium chloride (ratio of magnesium alcohol to 2.8:1), and stir After the magnesium chloride is completely dissolved, add 75mL of white oil and 75mL of silicone oil, stir and mix, and maintain at a temperature of 120°C for 1.5h to obtain a uniformly dispersed emulsion;

[0090] Through the emulsifier, under the condition of pressure of 0.5MPa and emulsifier speed of 3300r / min, spray the obtained emulsion into another stirred reactor containing 1600mL of hexane and cooled to -25°C in advance , keep the temperature of hexane not higher than -20°C, stir for 30 minutes, filter, wash with dry hexane, wash away the silicone oil and white oil, vacuum dry and sieve to obtain a spherical carrier with a size of 22 μm to 45 μm, its composition MgCl 2 2.54C 2 ...

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Abstract

The invention relates to a catalyst for polydiene synthesis and a preparation method thereof. The catalyst comprises a main catalyst and a cocatalyst, wherein the main catalyst comprises a spherical support, and an active component and phosphates on the spherical support; the spherical support is a magnesium chloride alcohol adduct or spherical silicon dioxide; and the active component is composed of one or more of titanium halides, vanadium halides, titanium oxyhalides and vanadium oxyhalides. The magnesium chloride alcohol adduct or spherical silicon dioxide is utilized to support the specific active component and phosphate compounds, so that the catalyst is in the regular spherical particle shape and has higher activity. Furthermore, di(2,6-di-tert-butyl-phenol) isobutyl aluminum, triisobutylaluminum, diisobutyl-2,6-di-tert-butyl phenol aluminum or tri((2,6-di-tert-butyl-phenol) aluminum is used as the cocatalyst. The polydiene prepared by using the catalyst has the advantages of low crystallinity, favorable morphology, favorable flowability and high trans content.

Description

technical field [0001] The invention belongs to the technical field of polymer synthesis, and in particular relates to a catalyst for polydiene synthesis and a preparation method thereof. Background technique [0002] High trans-1,4-polydiene, its monomers are more regularly arranged in the structure of trans-1,4- in the molecular chain of the material, which is easy to crystallize. This structure endows polydiene with many unique and excellent properties, making it widely used. For example, high trans-1,4-polyisoprene (TPI) can be used as shape memory functional materials, medical materials, plastics and modified rubber materials, etc., while high trans-1,4-polybutadiene Good crystallinity, when used as rubber, it has the advantages of large modulus, high hardness, good wear resistance, acid and alkali resistance and various solvents, and its tensile strength, elongation and elasticity are similar to styrene-butadiene rubber. [0003] Ziegler-Natta catalyst is currently t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F36/02C08F4/654C08F4/651C08F4/02C08F136/08
Inventor 张春雨张学全胡雁鸣白晨羲张贺新毕吉福代全权于琦周那丽华
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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