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Polyisoprene rubber alloy with core-shell structure and preparation method thereof

A polyisoprene and rubber alloy technology, applied in the field of polyisoprene synthesis, can solve problems such as unfavorable industrial production, polymer bonding, and lower crystallinity, and achieve favorable application, high activity, and improved processing performance Effect

Active Publication Date: 2017-05-17
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The above method can obtain composite rubber with better dynamic mechanical properties, but, because the reactivity ratio of butadiene and isoprene is very different, under very long polymerization time, what obtains is butadiene / isoprene Block copolymers or blends of isoprene and trans-polyisoprene, trans-butadiene is more prone to crystallization, so it does not have a large effect on the reduction of crystallinity and tends to cause polymer sticking , unfavorable to normal industrial production

Method used

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  • Polyisoprene rubber alloy with core-shell structure and preparation method thereof
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  • Polyisoprene rubber alloy with core-shell structure and preparation method thereof

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preparation example Construction

[0033] Correspondingly, the present application also provides a method for preparing the polyisoprene rubber alloy described above, comprising the following steps:

[0034] Mix isoprene, diisobutyl (2,6-di-tert-butylphenol) aluminum and the main catalyst for prepolymerization. After 0.5h to 5h, add butadiene for polymerization to obtain core-shell Structural polyisoprene rubber alloy;

[0035] The main catalyst includes: a spherical carrier and an active component loaded on the spherical carrier and a phosphate compound; the spherical carrier is magnesium chloride alcoholate or spherical silica; the active component It is one or more of halides of titanium, halides of vanadium, oxyhalides of titanium and oxyhalides of vanadium.

[0036]This application adopts a catalyst with high activity, so that the obtained polymer has good shape, good fluidity, and high trans content; this application adopts two-step polymerization, first prepares trans isoprene homopolymer under bulk con...

Embodiment 1

[0082] (1) carrier preparation

[0083] 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;

[0084] 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.

[0085] (2...

Embodiment 2

[0092] The preparation of the main catalyst is the same as in Example 1.

[0093] In a 500mL reactor fully dried and replaced with nitrogen, add 200mL of isoprene monomer (IP) at a molar ratio of Ti / IP=1×10 -4 , molar ratio Al / Ti=50, add diisobutyl (2,6 di-tert-butylphenol) aluminum and the main catalyst in sequence, fully stir for 1 hour at a temperature of 0°C for prepolymerization, and then add 4.32g For butadiene monomer, increase the reaction temperature to 30°C for polymerization, and react for 10 hours. During the reaction, measure the molar ratio of isoprene to butadiene monomer in the reaction liquid by chromatography every 2 hours, and add butadiene monomer The body maintains a molar ratio of IP / BD=25:1. After the reaction was completed, the unreacted isoprene monomer was vacuumed out, and the reaction was terminated with a 1% BHT-ethanol solution to obtain 70.0 g of polyisoprene alloy product. The monomer conversion rate was 51%, and the product reversed Formula-1...

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Abstract

The application provides a polyisoprene rubber alloy and a preparation method thereof. In the method, prepolymerization is carried out after mixing isoprene, diisobutyl (2,6-di-tert-butylphenol) aluminum and a main catalyst After 0.5h to 5h, butadiene is added for polymerization to obtain a polyisoprene rubber alloy with a core-shell structure; the main catalyst includes: magnesium chloride alcoholate or spherical silica spherical carrier; And the active components and phosphate compounds loaded on the spherical carrier. The invention controls the polymerization process conditions, adopts the staged polymerization method to first prepare the high trans 1,4-structure, and solves the fluidity problem in the processing process while ensuring the high trans-1,4-content of polyisoprene. Obtain high-performance polyisoprene alloy; and can fundamentally solve the polymer morphology control in bulk precipitation polymerization, avoiding the polymer modification process of trans-polyisoprene with isoprene and butadiene copolymerization Particle sticking occurs.

Description

technical field [0001] The invention belongs to the technical field of polyisoprene synthesis, in particular to a polyisoprene rubber alloy with a core-shell structure 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. Chinese patent documents with application numbers 95110352.0, 200610043556.4 and 201310206156.0 respectively disclose the preparation methods of TPI. The TPI prepared by the methods disclosed in these documents is easy to crystallize or has a high degree of crystallinity. The degree of crystallinity is above 30%. Plastic, its ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F236/08C08F236/06C08F136/08C08F2/02C08F4/649
Inventor 张春雨张学全胡雁鸣白晨曦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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