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Purification method for removing metal salt catalyst in ATRP (atom transfer radical polymerization) high-molecular product

A purification method and polymer technology, which is applied in the field of purification of metal salt catalysts in ATRP polymer products, can solve the problems of demanding mobile phase viscosity, consumption of a large amount of eluent, negative environmental impact, etc., and achieve the residual metal salt content Low, low equipment requirements, low environmental pollution effect

Inactive Publication Date: 2015-04-22
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although Al 2 o 3 Chromatographic column method and resin adsorption method are effective in removing metal salts, and the residual amount of metal salt catalyst is small, but the resin and Al 2 o 3 Both have irreversible adsorption to some polymers, resulting in low product yields. At the same time, this type of method has strict requirements on the viscosity of the mobile phase. The entire purification process consumes a large amount of eluent and takes time, while the traditional dissolution and precipitation method consumes a lot. Organic solvents that have a negative impact on the environment and are difficult to use for the purification of large quantities of ATRP products

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) CuBr / CuBr 2 As a catalytic system, use 2-bromomethyl methacrylate as an initiator to carry out atom transfer radical polymerization reaction of styrene monomer to obtain polystyrene as a polymer product, and dissolve 5 g of the product in 25 mL of anisole, Obtain polymer solution;

[0026] (2) Add 10 g of 200-mesh neutral alumina to the polymer solution obtained in step (1), and stir with a magnetic stirrer at a speed of 300 r / min for 15 min to make it evenly mixed;

[0027] (3) Filter the above mixed solution in a 6cm short-necked funnel equipped with medium-speed filter paper to obtain the crude filtrate;

[0028] (4) The crude filtrate is distilled under reduced pressure, the fraction is collected to reclaim the solvent anisole, and the concentrated filtrate is obtained;

[0029] (5) Add the concentrated filtrate of the step into 200mL of absolute ethanol, filter with suction to get the precipitate and continue to wash with absolute ethanol until the solution i...

Embodiment 2

[0032] (1) with CuCl / CuCl 2 As a catalytic system, the monomer 4-vinylpyridine was subjected to atom transfer radical polymerization reaction with benzyl chloride as the initiator to obtain the polymer product poly-4-vinylpyridine, and 1 g of the product was dissolved in 5 mL of isopropanol , to obtain a polymer solution;

[0033] (2) Add 10 g of 200-mesh neutral alumina to the polymer solution obtained in step (1), and stir with a magnetic stirrer at a speed of 300 r / min for 15 min to make it evenly mixed;

[0034] (3) Filter the above mixed solution in a 6cm short-necked funnel equipped with medium-speed filter paper to obtain the crude filtrate;

[0035] (4) The crude filtrate is distilled under reduced pressure, the fraction is collected to recover the solvent isopropanol, and the concentrated filtrate is obtained;

[0036] (5) Add the concentrated filtrate to 200mL of frozen ether, filter with suction to get the precipitate and continue to wash with frozen ether until t...

Embodiment 3

[0039] (1) CuBr / CuBr 2 As a catalytic system, benzyl chloride was used as an initiator to carry out atom transfer radical polymerization reaction on monomer styrene to obtain macromolecular initiator polystyrene, and 1 g of the product was dissolved in 5 mL of ethyl acetate to obtain a polymer solution ;

[0040] (2) Add 5g of activated carbon to the polymer solution obtained in step (1), stir with a magnetic stirrer at a speed of 300r / min for 5min to make it evenly mixed;

[0041] (3) Put the above mixed solution in a sand core and filter to obtain the crude filtrate;

[0042] (4) The crude filtrate is distilled under reduced pressure, the fraction is collected to recover the solvent ethyl acetate, and the concentrated filtrate is obtained;

[0043](5) Add the concentrated filtrate into 50mL of methanol, filter with suction to get the precipitate and continue to wash with methanol until the solution is colorless;

[0044] (6) The product was collected and vacuum-dried to c...

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Abstract

The invention relates to a purification method for removing a metal salt catalyst in an ATRP (atom transfer radical polymerization) high-molecular product, comprising the following steps of: dissolving an atom transfer radical polymerization ATRP reaction product in a solvent A to obtain high-molecular solution, then adding an adsorbent in the high-molecular solution, stirring and filtering to obtain a rough filtrate, and performing reduced pressure distillation to obtain the concentrated filtrate; dripping the concentrated filtrate aforementioned in a solvent B under the action of stirring, performing extraction filtration to obtain a precipitate, then washing, vacuum-drying, and then obtaining the product. The invention discloses a principle of realizing the separation between the high-molecular product and the metal salt catalyst by virtue of the solubility difference thereof in a solvent and the adsorption capacity difference thereof for an adsorbent, optimizes a purification process, and can finish the operation in conventional conditions without the need to use cumbersome devices such as a chromatographic column; the purification method is low in requirements on equipment, simple and convenient in the whole purification process, and less in environmental pollution; and moreover, the product yield is greater than 85%, the content of residual metal salts after purification is low, and the mass fraction is less than 0.0004%.

Description

technical field [0001] The invention belongs to the field of polymer purification methods, in particular to a purification method for removing metal salt catalysts in ATRP polymer products. Background technique [0002] Atom Transfer Radical Polymerization (ATRP) is a novel living radical polymerization method. Compared with other traditional free radical polymerizations, ATRP has milder reaction conditions, a wide range of applicable monomers, and strong molecular design capabilities. It is an important means of synthesizing polymers with specific structures and properties. Atom transfer radical polymerization can achieve uniform chain growth to obtain low-dispersion polymers, which mainly depends on the transition metal catalyst (common catalysts are CuCl / CuCl 2 , CuBr / CuBr 2 and FeCl 2 / FeCl 3 etc.), the catalyst makes an equilibrium between the active growing polymer chains and the dormant inactive polymer chains. Since the dormant polymer is more dominant in this b...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F6/08
Inventor 何瑾馨张韡董霞王振华
Owner DONGHUA UNIV