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Cyclic polystyrene and preparation method thereof

A polystyrene and cyclic technology, which is applied in the field of cyclic polystyrene and its preparation, can solve the problems of harsh reaction conditions, difficult separation, and low cyclization efficiency of anion methods, so as to avoid the increase of coupling by-products, high The effect of molecular weight and high yield

Inactive Publication Date: 2018-08-31
SHENZHEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the reaction conditions of the anion method are harsh, the cyclization efficiency is relatively low, and the unreacted linear precursor and the cyclic product have similar chain sizes. It is difficult to separate by traditional sedimentation fractionation or preparative chromatography, and requires tedious critical liquid chromatography. [Lee, H.C. et al. Macromolecules 2000, 33, 8119-8121]
[0003] Active atom transfer radical polymerization (ATRP) technology and click chemistry provide effective means for the synthesis of various polymers with special structures. However, in the current synthesis process of cyclic polymers such as cyclic polystyrene, it is difficult to simultaneously Taking into account the high yield, high purity and high molecular weight of cyclic polymers

Method used

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  • Cyclic polystyrene and preparation method thereof
  • Cyclic polystyrene and preparation method thereof
  • Cyclic polystyrene and preparation method thereof

Examples

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Embodiment 1

[0058] A preparation method of cyclic polystyrene, comprising:

[0059] (1) 43.6mmol of styrene, 0.15mmol of cuprous bromide, 0.015mmol of copper bromide and 0.30mmol of N,N,N',N,'N"-pentamethyldiethylenetriamine Add in the reaction tube, evacuate under freezing to remove water and oxygen, then return the temperature of the mixture to room temperature, obtain the first mixed solution of dissolving (hereinafter referred to as "freezing water and oxygen removal").Add 0.15mmol of iso Propargyl bromobutyrate was subjected to a polymerization reaction at room temperature for 8 hours, and the reaction tube was placed in a liquid nitrogen tank to terminate the polymerization reaction to obtain a polymerization product.

[0060] Purification: first dilute the obtained polymer product with dichloromethane, and pass through an alkaline aluminum column to remove copper salts (cuprous bromide, copper bromide), add methanol to the solution obtained after passing through the column, and set...

Embodiment 2

[0067] A preparation method of cyclic polystyrene, comprising:

[0068] (1) Add 43.6mmol of styrene, 0.30mmol of cuprous bromide, 0.030mmol of copper bromide and 0.30mmol of N,N,N',N,'N"-pentamethyldiethylenetriamine Add in the reaction tube to obtain the first mixed solution, freeze to remove water and oxygen.Add 0.30mmol propargyl isobromobutyrate to it, carry out polymerization reaction at room temperature for 8 hours, and place the reaction tube in a liquid nitrogen tank to terminate This polymerization reaction yields a polymer product.

[0069] Purification: first dilute the obtained polymer product with dichloromethane, and pass through an alkaline aluminum column to remove copper salts (cuprous bromide, copper bromide), add methanol to the solution obtained after passing through the column, and settle out the crude polymer; Dissolve the crude polymer product in toluene, add n-heptane, settle and remove high-molecular-weight by-products, repeat the dissolution-sediment...

Embodiment 3

[0077] A preparation method of cyclic polystyrene, comprising:

[0078] (1) 43.6mmol of styrene, 0.11mmol of cuprous bromide, 0.011mmol of copper bromide and 0.11mmol of N,N,N',N,'N"-pentamethyldiethylenetriamine Add in the reaction tube, vacuumize under freezing to remove water and oxygen, then return the temperature of the mixture to room temperature to obtain the first mixed solution (hereinafter referred to as "freezing water and oxygen removal") that dissolves. Add 0.11mmol of iso Propargyl bromobutyrate was subjected to a polymerization reaction at room temperature for 16 hours, and the reaction tube was placed in a liquid nitrogen tank to terminate the polymerization reaction to obtain a polymerization product.

[0079] Purification: first dilute the obtained polymer product with dichloromethane, and pass through an alkaline aluminum column to remove copper salts (cuprous bromide, copper bromide), add methanol to the solution obtained after passing through the column, a...

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Abstract

The invention provides a preparation method of cyclic polystyrene. The method comprises the steps that firstly, linear polystyrene is prepared through an ATRP reaction and then made into end-group azidation linear polystyrene; secondly, azidation linear polystyrene is cyclized into cyclic polystyrene through a click chemistry method, and the cyclization process is controlled, wherein the rate of adding azidation linear polystyrene dropwise is controlled within 0.001-0.0025 mL / min, the total concentration of azidation linear polystyrene in a reaction system after dropwise addition is 0.5-5 mmol / L, and the temperature of the cyclization reaction is 25-50 DEG C. Prepared cyclic polystyrene can have high purity, high yield and high molecular weight at the same time. The invention further provides prepared cyclic polystyrene with the high molecular weight and purity.

Description

technical field [0001] The invention relates to the technical field of polymer materials, in particular to a cyclic polystyrene and a preparation method thereof. Background technique [0002] Cyclic polymers are macromolecular compounds without chain ends, which have different properties from traditional linear polymers. Due to the entropy factor, the synthesis of cyclic polymers is more difficult than that of linear polymers, and there are fewer research reports on them. Taking cyclic polystyrene as an example, it is usually obtained by a ring-closing strategy, such as first obtaining a linear precursor through anionic polymerization, and then connecting the two active ends of the precursor through a coupling agent [Roovers, J et al. Macromolecules 1983, 16, 843-849.]. However, the reaction conditions of the anion method are harsh, the cyclization efficiency is relatively low, and the unreacted linear precursor and the cyclic product have similar chain sizes. It is diffic...

Claims

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Application Information

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IPC IPC(8): C08F112/08C08F8/48C08F8/30
CPCC08F8/30C08F8/48C08F112/08
Inventor 阎志超南图高福
Owner SHENZHEN UNIV
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