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Method for removing cupric salt catalyst from product of ATRP

A reaction product and catalyst technology, applied in the field of polymer chemistry, can solve the problems of consuming organic solvent yield, low purification yield, high Cu residue, etc.

Inactive Publication Date: 2009-09-02
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the literature on the removal method of catalyst Cu generally uses Al 2 o 3 Column method and dissolution precipitation method, although Al 2 o 3 The column method has a better effect of removing Cu, and the residual amount is less, but the Al 2 o 3 Can cause irreversible adsorption to some polymers, resulting in low purification yields
The dissolution and precipitation method will consume a large amount of organic solvent and the yield is also low, and the Cu residue is high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Add 50 ml of dichloromethane to 1.000 g of CuCl-catalyzed polylactic acid and polymethyl methacrylate ATRP reaction mixed product (Mn=10000) to fully dissolve, transfer the product solution into a separatory funnel, and use 100 ml of 5% HCl aqueous solution successively , 100ml of 5% HCl aqueous solution, and 100ml of distilled water to extract 3 times. The organic phase filtrate was collected, concentrated under reduced pressure, 50ml of methanol was added to precipitate the product, and the solution was washed until the solution was colorless and neutral. The collected product was vacuum-dried to constant weight to obtain a purified polymer product with a yield of 80% and residual Cu=0.8ppm.

Embodiment 2

[0015] Add 40ml of 1,2 dichloroethane to 1.000g of CuBr-catalyzed polylactic acid and polystyrene ATRP reaction mixed product (Mn=20000) to fully dissolve, transfer the product solution into a separatory funnel, and use 10% HCl aqueous solution successively 100ml, 50ml of 5% HCl aqueous solution, and 50ml of 5% HCl aqueous solution were extracted three times. Collect the organic phase filtrate, concentrate under reduced pressure, add 30ml of methanol to precipitate the product, and wash until the solution is colorless and neutral. The collected product is vacuum-dried to constant weight to obtain a purified polymer product with a yield of 85% and residual Cu=1.5ppm.

Embodiment 3

[0017] Add 20ml of chloroform to 1.000g of CuCl-catalyzed polylactic acid and polymethyl methacrylate ATRP reaction mixed product (Mn=15000) to fully dissolve, transfer the product solution into a separatory funnel, and use distilled water 50ml, 5% 50 ml of HCl aqueous solution and 50 ml of 5% HCl aqueous solution were extracted three times. The organic phase filtrate was collected, concentrated under reduced pressure, 20ml of methanol was added to precipitate the product, and the solution was washed until the solution was colorless and neutral. The collected product was vacuum-dried to constant weight to obtain a purified polymer product with a yield of 82% and residual Cu=1.5ppm.

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PUM

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Abstract

The invention belongs to a method for purifying the product of atom transfer radical polymerization (ATRP) and particularly relates to a method for removing a cupric salt catalyst from the product of ATRP. The process of the method comprises the following steps of: dissolving a product of the ATRP in a solvent I; extracting the product with an extract solution for three times; concentrating the product under reduced pressure; adding a solvent II into the concentrated product to precipitate the product; washing the product till the solution is colorless and neutral; collecting the product and drying the product under vacuum till the weight of the product is constant; and obtaining the purified ATRP polymerization product. The method has the advantages that: the purification process is simple, environmental pollution is little, the product yield is more than 80 percent, and the residual Cu content after purification is less than 2ppm.

Description

technical field [0001] The invention relates to a method for removing an ATRP reaction product copper salt catalyst, belonging to the technical field of polymer chemistry. Background technique [0002] Atom transfer radical polymerization (ATRP) is a new polymerization method developed in recent years. The ATRP initiation system is composed of three parts: halide initiator / low-valent transition metal salt / electron donor ligand (RX / MtnXn / Lm). Common low-valent transition metal salt catalysts include CuCl, FeCl 2 、RuCl 2 Among them, CuCl is more commonly used. Compared with other polymerization methods, ATRP can make the molecular weight distribution of the obtained copolymer narrower and better controllable, so it has become an important means of polymer structure design. Compared with living ionic polymerization, ATRP has more suitable monomers, mild reaction conditions, easy control, and great industrialization potential. In addition, the polycondensation product can b...

Claims

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Application Information

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IPC IPC(8): C08F6/08C08F6/12
Inventor 刘晓宁魏荣卿沈珺
Owner NANJING UNIV OF TECH
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