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Preparation method of multi-arm acrylate block copolymer

A technology of block copolymer and acrylate, applied in the field of preparation of multi-arm acrylate block copolymer, can solve the problems of high realization difficulty and complex synthesis of hyperbranched macromolecular initiators, and achieves simplified process and realization difficulty, The effect of improved regularity and improved performance

Inactive Publication Date: 2015-09-09
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] These methods can be used to synthesize multi-arm block polymers, and they all prepare macromolecules with complex structures as initiators to synthesize multi-arm polymers. They belong to the first-nucleus-back-arm method, and the synthesis of hyperbranched macromolecular initiators is relatively Complex implementation is relatively difficult

Method used

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  • Preparation method of multi-arm acrylate block copolymer
  • Preparation method of multi-arm acrylate block copolymer
  • Preparation method of multi-arm acrylate block copolymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Preparation of hydroxyl-terminated polybutyl acrylate-b-polymethyl methacrylate (HO-PBA-b-PMMA), the molecular weight is 40600, and the structure is:

[0026]

[0027] Wherein, m=200, n=150.

[0028] Add 60.00 g of butyl acrylate, 0.5604 g of hydroxybutyl α-bromoisobutyrate, CuBr 2 0.04194g and pentamethyldivinyltriamine 0.6490g, Sn(EH) 2 1.517g and 30.00g of solvent toluene, after mixing evenly, bubbling with nitrogen gas, reacting in an oil bath at 70°C for 210min, after the conversion rate reaches 82.7%, weighed 35.16g of methyl methacrylate, 18.00g of toluene and Sn(EH) 2 1.138g was added into the reaction bottle with a syringe, and the reaction was stopped after 255min. The product was passed through a neutral alumina chromatography column to remove the catalyst in the polymer, and methanol was precipitated after rotary evaporation, and then dried in a vacuum oven at 50°C until constant 79 g of the product was obtained with a yield of 83%.

[0029] (2) P...

Embodiment 2

[0033] (1) Preparation of hydroxyl-terminated polyethylacrylate-b-polybutylmethacrylate (HO-PEA-b-PBMA), the molecular weight is 32000, and the structure is:

[0034]

[0035] Wherein, m=200, n=85.

[0036]Add 60.00 g of ethyl acrylate, 0.7173 g of α-bromoisobutyrate 0.7173 g, CuBr 2 0.05369g and pentamethyldivinyltriamine 0.8308g, Sn(EH) 2 1.942g and 30.00g of solvent toluene, after mixing evenly, bubbling with nitrogen gas, reacting in an oil bath at 70°C for 210min, after the conversion rate reaches 85%, 36.00g of methyl methacrylate, 18.00g of toluene and Sn(EH) 2 Add 0.8264g into the reaction bottle with a syringe, stop the reaction after 260min, pass the product through a neutral alumina chromatography column, remove the catalyst in the polymer, and precipitate methanol after rotary evaporation, and then dry it in a vacuum oven at 50°C until constant Weight, to obtain product 75g, yield 78%.

[0037] (2) Preparation of multi-arm PEA-b-PBMA

[0038] NCO / OH=1.1:1 ...

Embodiment 3

[0041] (1) Preparation of hydroxyl-terminated polymethyl acrylate-b-polyisooctyl acrylate (HO-PMA-b-PEHA), the molecular weight is 21000, and the structure is:

[0042]

[0043] Wherein, m=100, n=68.

[0044] Add 60.00 g of methyl acrylate, 1.668 g of hydroxybutyl α-bromoisobutyrate, CuBr 2 0.06251g and pentamethyldivinyltriamine 0.967g, Sn(EH) 2 2.261g and 30.00g of solvent toluene, after mixing evenly, bubbling with nitrogen gas, reacting in an oil bath at 70°C for 250min, after the conversion rate reached 81%, weighed 86.57g of isooctyl acrylate, 43.00g of toluene and Sn (EH) 2 Add 1.525g into the reaction bottle with a syringe, stop the reaction at 70°C for 300min, pass the product through a neutral alumina chromatography column, remove the catalyst in the polymer, and precipitate methanol after rotary evaporation, and then place it in a vacuum oven at 50°C After drying to constant weight, 103 g of the product was obtained with a yield of 70.2%.

[0045] (2) Prepara...

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Abstract

The invention relates to a preparation method of multi-arm acrylate block copolymer. The preparation method includes the steps of preparing hydroxyl terminated acrylate macromolecular initiator, preparing hydroxyl terminated acrylate block copolymer and preparing the multi-arm acrylate block copolymer. The preparation method has the advantages that an ARGET ATRP method is adopted to synthesize the multi-arm acrylate block copolymer, so that composition and structure of arms can be controlled accurately; dispersity of the copolymer is controlled through ATRP, so that regularity of the block copolymer is improved greatly, and product yield is increased; polymerization reaction can be performed in relatively open space, amount of catalyst is smaller than 500ppm, and the product can be used directly without removing the catalyst, and the preparation method is high in efficiency and low in cost as compared with conventional methods; reaction of hydroxy and isocyanate base is utilized to connect the arms on polyisocyanate in a keyed manner to form a multi-arm structure using polyisocyanate as the center and acrylate block copolymer as the arms; an arm-first core-second method is utilized to simplify the process and implementation.

Description

technical field [0001] The invention belongs to the field of chemical materials and relates to a preparation method of a multi-arm acrylate block copolymer. Background technique [0002] Block copolymers are composed of two or more polymer segments with different chemical structures. According to the number of monomers that make up block copolymers, they can be divided into two-block, three-block, and multi-block. Duan and so on. It can combine the excellent properties of various polymers to obtain functional polymer materials with superior performance. [0003] There are many ways to synthesize block copolymers, including living anionic polymerization, living cationic polymerization, group transfer polymerization, controlled / living free radical polymerization, etc. As a special linear copolymer, block copolymers are different from blends and graft copolymers in structure and properties. Its glass transition temperature is determined by the polymer with a lower temperatur...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G18/63C08F293/00
CPCC08F120/14C08F120/18C08F120/44C08F293/005C08G18/0823C08G18/348C08G18/4063C08G18/48C08G18/4812C08G18/6225C08G18/6245C08G18/6262C08G18/633C08G18/638C08G18/6511C08G18/6607C08G18/6692C08G18/7621
Inventor 李坚刘新孙仪琳任强汪称意
Owner CHANGZHOU UNIV
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