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Hydroxyl-terminated polyacrylate oligomer as well as preparation method and application thereof

A technology of hydroxyl-terminated polyacrylic acid and polyacrylates, which is applied in the preparation of carboxylates by oligomerization, organic chemistry, etc., and can solve problems such as adverse effects of application

Active Publication Date: 2013-03-13
溧阳常大技术转移中心有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

They all use primary alcohol amines to modify polymers, and the residual active hydrogen on the resulting products may have an adverse effect on the application in polyurethane

Method used

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  • Hydroxyl-terminated polyacrylate oligomer as well as preparation method and application thereof
  • Hydroxyl-terminated polyacrylate oligomer as well as preparation method and application thereof
  • Hydroxyl-terminated polyacrylate oligomer as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Example 1: (Preparation of polybutyl acrylate with a molecular weight of 500)

[0045] Polymerization formula: initiator (ethyl α-bromoisobutyrate): monomer (butyl acrylate): catalyst: ligand = 1: 2.4: 0.048: 0.096 (molar ratio), and then add 25% of the system mass. Ethyl acetate was used as solvent.

[0046] Polymerization step: add 128.94g (0.66mol) initiator ethyl α-bromoisobutyrate, 202.37g (1.58mol) monomer butyl acrylate, 4.59g (0.032mol) catalyst CuBr in a 500ml four-necked flask, 11.05g (0.064mol) ligand PMDETA, 86.74g solvent ethyl acetate, mix well. The system was evacuated and filled with nitrogen, and the reaction was stirred for 8 hours under an oil bath at 70°C. After the reaction is completed, after removing the catalyst and the solvent, a light yellow transparent and slightly viscous product can be obtained, the product mass is 304.4 g, and the yield is 91.9%. GPC test was performed on the product, and the number-average molecular weight of polybutyl ...

Embodiment 2

[0047] Embodiment 2: (the preparation of molecular weight 500 hydroxyl-terminated polybutyl acrylate)

[0048] Modified formula: polybutylacrylate:N-methylmonoethanolamine:triethylamine=1:25:5 (molar ratio). Modification step: add 19.63g (0.034mol) polybutyl acrylate in Example 1, 69.4g (0.925mol) N-methylmonoethanolamine, 19.2g (0.190mol) triethylamine into a 150ml four-necked flask, mix well . The system was evacuated and filled with nitrogen, and the reaction was stirred for 8 hours in an oil bath at 90°C. After the reaction, pickling was performed, and the oil layer was extracted after washing with anhydrous MgSO. 4 After drying, it was passed through a column, and finally the solvent was removed to obtain 6.7 g of a light yellow, viscous and transparent product. Yield 34%. GPC test was performed on the product, and the number-average molecular weight of the hydroxyl-terminated polybutylacrylate was Mn=642, and the molecular weight distribution PDI=1.09. The hydroxyl-...

Embodiment 3

[0049] Example 3: (Preparation of polybutyl acrylate with a molecular weight of 1000)

[0050] Polymerization formula: initiator (ethyl α-bromoisobutyrate): monomer (butyl acrylate): catalyst: ligand=1:7:0.07:0.014 (molar ratio), then add 25% of the system mass. Ethyl acetate was used as solvent.

[0051] Polymerization step: add 39.42g (0.20mol) initiator ethyl α-bromoisobutyrate, 179.91g (1.405mol) monomer butyl acrylate, 2.02g (0.014mol) catalyst CuBr in a 500ml four-necked flask, 4.83g (0.028mol) ligand PMDETA, 67g solvent ethyl acetate, mix well. The system was evacuated and filled with nitrogen, and the reaction was stirred for 8 hours under an oil bath at 70°C. After the reaction is completed, after removing the catalyst and the solvent, a light yellow transparent and slightly viscous product can be obtained, the product quality is 167.4 g, and the yield is 93%. The product was tested by GPC, and the number-average molecular weight of polybutyl acrylate was obtained ...

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Abstract

The invention relates to a preparation method of hydroxyl-terminated polyacrylate oligomers, which comprises the following steps: preparing low molecular weight polyacrylate oligomers with controllable molecular weight, such as polybutylacrylate, polyethylacrylate, oly(isooctyl acrylate), polymethyl methacrylate, a block copolymer of butyl acrylate and methyl methacrylate, a block copolymer of themethyl methacrylate and dimethylaminoethyl methacrylate, and the like by adopting atom transfer radical polymerization (ATRP) and using organic halide as an initiating agent; and then carrying out terminal group modification on the polymers by N-methylethanolamine to obtain the hydroxyl-terminated polyacrylate oligomers with controllable molecular weight. The prepared hydroxyl-terminated polyacrylate oligomers can be used for the production of polyurethane. Because the molecular weight of the hydroxyl-terminated polyacrylate oligomers is controllable, a polyurethane material with special performance can be prepared.

Description

technical field [0001] The invention belongs to the field of chemical materials, and relates to a method for synthesizing a hydroxyl-terminated polyacrylate oligomer by utilizing atom transfer radical polymerization (ATRP). raw materials. Background technique [0002] Atom transfer radical polymerization (ATRP) is a new method of polymer synthesis. Different from traditional free radical polymerization, ATRP can control the molecular weight of polymers and synthesize polymers with various predetermined structures (block copolymers, graft copolymers, star polymers, comb polymers, hyperbranched polymers, cross-linked network polymers, end-functional polymers, etc.). [0003] The research on the initiating system of ATRP polymerization showed that all haloalkanes containing inducing conjugation group at the α-position could initiate ATRP reaction. The ATRP product prepared from this initiator has an alkyl moiety on the initiator at one end and a halogen on the initiator at t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/465C07C69/675C08F120/12C08F220/10C08F8/32C08G18/62
Inventor 李坚甄颖朋俞强崔英山岸雅幸池田裕治
Owner 溧阳常大技术转移中心有限公司
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