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1,3-piperlene alternating copolymer based cyclized compound and preparation method thereof

A technology of alternating copolymers and piperylene, which is applied in the field of cyclization and its preparation, can solve the problems of difficulty in the preparation of alternating copolymers, great differences in polyreactivity ratio, and improved branched structure, and achieve high heat resistance , Narrow molecular weight distribution and high degree of cyclization

Pending Publication Date: 2021-10-12
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, from this aspect, the higher the content of alternating sequence structure of dienes, the easier it is to cyclize, but the preparation of alternating copolymers is extremely difficult.
When styrene and butadiene and styrene-isoprene anionic copolymerize, due to the great difference in the rate of segregation, a gradual block copolymer will be formed. Although the degree of randomization can be improved to a certain extent, the degree of alternation is limited. At the same time, the branched structure in the product is greatly improved, which will directly lead to side reactions such as crosslinking or intermolecular cyclization in the subsequent cyclization reaction process.

Method used

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  • 1,3-piperlene alternating copolymer based cyclized compound and preparation method thereof
  • 1,3-piperlene alternating copolymer based cyclized compound and preparation method thereof
  • 1,3-piperlene alternating copolymer based cyclized compound and preparation method thereof

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preparation example Construction

[0068] A second aspect of the present invention provides a method for preparing a cyclized product based on piperylene alternating copolymers, the method comprising the following steps:

[0069] (1) using an organic alkali metal as an initiator to copolymerize piperylene monomers and styrene monomers shown in formula (8) in a solvent, and then terminate the polymerization with water;

[0070] (2) Contacting the copolymerization product obtained in step (1) with a cyclization catalyst to carry out a cyclization reaction.

[0071]

[0072] Among them, R 1 and R 2 The meaning of is as above. The styrene-based monomer may be, for example, styrene, methylstyrene, or diphenylethylene.

[0073] The mechanism of the method of the present invention can be tried to be explained by the following formula.

[0074]

[0075] Among them, the composition ratio of piperylene / styrene-based monomer anionic copolymerization unit and the data and kinetic characteristics of the reactivity...

specific Embodiment approach

[0098] According to a specific embodiment of the present invention, the production process of the cyclized styrene-piperylene alternating copolymer comprises: adding piperylene monomer and styrene monomer into cyclohexane in an equimolar ratio, stirring and dissolving Then add the regulator tetrahydrofuran, then add the initiator butyllithium to initiate, control the temperature at 60-80°C, and carry out the polymerization reaction in the polymerization kettle for 0.5-3h. After the molecular weight and viscosity of the polymerization reaction product meet the requirements, add the terminator water The polymerization reaction is stopped, and at the same time, the temperature is lowered to 20-40° C., and the material is transferred to the cyclization kettle. Add a cyclization reaction catalyst to carry out the cyclization reaction. When the cyclization reaction has progressed to a certain extent, add a cyclization reaction terminator, enter the washing tower and add water to full...

Embodiment 1

[0105] Add piperylene and diphenylethylene monomers into cyclohexane (3.0mL per 0.4mL monomer) in equimolar ratio, stir and dissolve, add regulator tetrahydrofuran (1mg / 100g monomer), and then add initiator Initiated by n-butyllithium (3.0mmol / L), the temperature was controlled at 70°C, and the polymerization reaction was carried out in the polymerization tank for 1 hour to obtain a prepolymer. The measured number average molecular weight of the prepolymer is 100,000, the molecular weight distribution is 1.04, the structure content of 1,4-piperylene is 85%, and the glass transition temperature is 88°C. At this point, water as a terminator was added to the polymerization kettle to stop the polymerization reaction, and at the same time, the temperature was lowered to 30° C., and the product was transferred to the cyclization kettle. Add the cyclization reaction catalyst to carry out the cyclization reaction of xylene sulfonic acid (1g / 100g monomer) for 5 hours, add the cyclizati...

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Abstract

The invention provides a 1,3-piperlene alternating copolymer based cyclized compound and a preparation method thereof, the 1,3-piperlene alternating copolymer based cyclized compound contains a cyclized structure unit shown in the following formula (1) and / or a cyclized structure unit shown in the following formula (2), the number-average molecular weight of the 1,3-piperlene alternating copolymer based cyclized compound is 1000-1000000, the total amount of the cyclized structural unit as shown in the formula (1) and the cyclized structural unit as shown in the formula (2) accounts for 80-100wt% of the total amount of the cyclized structural unit. The 1,3-piperlene alternating copolymer based cyclized compound has the advantages of high cyclization degree (up to 100%), no gel, narrow molecular weight distribution (less than 1.3) and the like, and has excellent comprehensive properties such as high Tg, high heat resistance, high transparency, low moisture absorption characteristic and the like, so that the 1,3-piperlene alternating copolymer based cyclized compound can be used as an optical and high-grade resin material.

Description

technical field [0001] The invention relates to a cyclization product based on piperylene alternating copolymers and a preparation method thereof, more specifically, to a high degree of cyclization, high heat resistance, no gel, narrow distribution and controllable piperylene alternation Copolymer cyclization product and its preparation method. Background technique [0002] Polymers of conjugated diolefins, such as polybutadiene rubber, polyisoprene rubber, solution polystyrene butadiene rubber and other prepolymers, are often introduced into rigid and thermally stable fused ring structures through simple and efficient cationic cyclization reactions And for optical materials. The cyclization of conjugated olefin polymers is generally carried out under the action of Lewis acid catalysts, and the intramolecular cyclization reaction is carried out according to the cationic mechanism, so that the heat resistance can be greatly improved. Since this type of reaction can transfor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F236/10C08F212/32C08F8/48C08F2/42C08F4/48C08F212/08C08F212/12
CPCC08F236/10C08F212/32C08F8/48C08F212/08C08F212/12C08F2/42C08F4/48C08F4/484
Inventor 刘坤夏金魁李安邱旭
Owner CHINA PETROLEUM & CHEM CORP
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