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Process for preparing halogen-free ATRP products

A substance and compound technology, applied in the field of transition metal complexes and transition metal removal, can solve the problems of increasing the concentration of copper removal ligands, unable to economically expand large industrial production capacity, etc., and achieve the effect of rapid processing

Inactive Publication Date: 2011-08-17
EVONIK ROEHM GMBH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the disadvantage is on the one hand the very high ligand concentration which can stain the product and additionally make copper removal more difficult
This approach cannot be scaled economically to large industrial production volumes

Method used

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  • Process for preparing halogen-free ATRP products

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0082] In a double-jacketed vessel equipped with a stirrer, calorimeter, reflux cooler, nitrogen inlet tube and dropping funnel, the 2 - 15 g of n-butyl acrylate, 15.5 g of butyl acetate, 0.2 g of copper(I) oxide and 0.5 g of PMDETA were introduced under atmosphere. The solution was stirred at 60 °C for 15 min. Then 0.49 g of 1,4-butanediol-bis-(2-bromo-2-methylpropionate) were added at the same temperature. The polymerization time was stirred at 70° C. for 4 hours. After about 5 min of introducing atmospheric oxygen to terminate the reaction, 0.6 g of n-dodecylmercaptan was added. The previously green solution automatically turned red and a red precipitate precipitated out. Filtration is carried out by means of overpressure filtration. The filter cake turned black within hours. Finally the average molecular weight and the molecular weight distribution of the polymers in the filtrate are determined by GPC-measurement. The copper content was then determined from the dried...

Embodiment 2

[0087] In a double-jacketed vessel equipped with a stirrer, calorimeter, reflux cooler, nitrogen inlet tube and dropping funnel, the 2 - 10 g of methyl methacrylate, 15.8 g of butyl acetate, 0.2 g of copper(I) oxide and 0.5 g of PMDETA were introduced under atmosphere. The solution was stirred at 60 °C for 15 min. Then 0.47 g of 1,4-butanediol-bis-(2-bromo-2-methylpropionate) was added at the same temperature. The polymerization time was stirred at 70° C. for 4 hours. After introducing air oxygen for about 5 min to terminate the reaction, 0.6 g of n-dodecylmercaptan was added. The previously green solution automatically turned red and a red precipitate precipitated out. Filtration is carried out by means of overpressure filtration. The filter cake turned black within hours. Finally the average molecular weight and the molecular weight distribution of the polymers in the filtrate are determined by GPC-measurement. The copper content was then determined from the dried filt...

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Abstract

The present invention relates to the in situ removal of terminal halogen atoms from polymer chains which have been prepared by means of atom transfer radical polymerization, and to the simultaneous removal of transition metals from polymer solutions.

Description

technical field [0001] The present invention relates to the in situ removal of terminal halogen atoms from polymer chains produced by means of atom transfer radical polymerization (hereinafter referred to as ATRP). Additionally, the present invention includes a method for removing transition metals from polymer solutions. In particular, it concerns the removal of transition metal complexes in amounts not exceeding 1000 ppm. In particular, it concerns the removal of mainly copper-containing transition metal complexes from polymer solutions after the end of the atom transfer radical polymerization reaction. [0002] A very particular aspect of the invention consists in the simultaneous removal of terminal halogen atoms from the polymer chain, optionally functionalization of the polymer termini, by means of precipitation in one method step by adding reagents Removal of the transition metal compound and salt formation of the ligand previously coordinated to the transition metal ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F6/02C08F2/38C08F8/26C08F8/34C08F220/10
CPCC08F2438/01C08F120/18C08F2/38C08F6/02C08F220/18C08F8/26C08F2810/40C08F8/34C08F220/1804C08F120/14C08F220/10
Inventor S·巴尔克G·勒登E·奥陶斯
Owner EVONIK ROEHM GMBH