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Method for preparing soluble crosslinked polystyrene uniform branch point distribution

A technology of cross-linked polystyrene and uniform distribution is applied in the field of preparation of cross-linked polystyrene and achieves the effects of mild preparation conditions, convenient synthesis and simple synthesis conditions

Active Publication Date: 2016-03-16
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although it has been reported that polymers can be prepared by free radical coupling reactions, there are few reports on the preparation of crosslinked polymers by carbon free radical coupling reactions

Method used

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  • Method for preparing soluble crosslinked polystyrene uniform branch point distribution
  • Method for preparing soluble crosslinked polystyrene uniform branch point distribution
  • Method for preparing soluble crosslinked polystyrene uniform branch point distribution

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] The synthesis of embodiment 1 polyamine ligand TPMA

[0042] Dissolve 16.4 g of 2-chloromethylpyridine hydrochloride (0.1 mol) in 40 mL of deionized water, cool in an ice bath, and slowly add 20 mL of aqueous solution in which 0.1 mol of sodium hydroxide is dissolved, and the solution turns pink. 80 mL of a DCM solution containing 5.4 g of 2-(aminomethyl)pyridine (0.05 mol) was added and warmed to room temperature. Add 20 mL of aqueous solution dissolved with 0.1 mol of sodium hydroxide with a micro-injector, and drop it in 50 hours. Stop the reaction, wash the organic phase with 3×10 mL of 15% NaOH aqueous solution, combine the organic phases, dry over anhydrous magnesium sulfate, filter, and concentrate. The product was extracted with diethyl ether in a boiling state, the insoluble matter was removed, cooled, the product was crystallized in diethyl ether, and filtered. The recrystallization was continued for 3 times to obtain pale yellow needle crystals with a yield...

Embodiment 2

[0043] The synthesis of embodiment 2 polyamine ligand TPEN

[0044] Dissolve 13.12 g of 2-chloromethylpyridine hydrochloride (0.08 mol) in 30 mL of deionized water, cool in an ice bath, and slowly add 15 mL of aqueous solution in which 0.08 mol of sodium hydroxide is dissolved, and the solution turns pink. Add 60 mL of a DCM solution containing 1.2 g of ethylenediamine (0.02 mol) and warm to room temperature. Add 15 mL of aqueous solution dissolved with 0.08 mol of sodium hydroxide with a micro-injector, and drop it in 50 hours. Stop the reaction, wash the organic phase with 3×10 mL of 15% NaOH aqueous solution, combine the organic phases, dry over anhydrous magnesium sulfate, filter, and concentrate. The product was extracted with diethyl ether in a boiling state, the insoluble matter was removed, cooled, the product was crystallized in diethyl ether, and filtered. The recrystallization was continued for 3 times to obtain pale yellow needle crystals with a yield of 37%. 1 ...

Embodiment 3

[0045] The synthesis of embodiment 3 initiator 3a

[0046] 2.7g 1,1,1-trimethylol-propane (2×10 -2 mol), 8mL triethylamine (6×10 -2 mol), 50mL of DCM were mixed, placed in a 250mL three-necked flask, and cooled in an ice bath. Will contain 8.2mL2-bromo-2-methylpropionyl bromide (6.6×10 -2 mol) of DCM solution (50 mL) was dropped into a three-necked flask, and after 1 hour, a white precipitate appeared, warmed up to room temperature (25° C.), and stirred overnight. Filter, wash the filtrate three times with 50mL1mol / LHCl solution, saturated NaHCO 3 Wash three times with aqueous solution, three times with 50mL deionized water, once with 50mL saturated NaCl, anhydrous MgSO 4 Let dry overnight. After filtration and concentration, a yellow viscous liquid was obtained. The crude product was recrystallized twice from methanol, filtered and dried under vacuum at 40°C overnight to obtain white crystals. 1 HNMR (400MHz, CDCl 3 )δ (ppm): 4.19 (6H, s, CH 2 -O-C=O),1.94(18H,s,O=C-...

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Abstract

The invention relates to preparation of crosslinked polystyrene, and aims to provide a method for preparing soluble crosslinked polystyrene uniform branch point distribution. The method comprises the following steps: adding multi-arm polystyrene containing a bromine end group, copper powder and polybasic amine ligands into a reactor holding a solvent; stirring after deoxygenation; conducting reaction to obtain soluble crosslinked polystyrene uniform branch point distribution. The method has the advantages that the synthesis conditions are simple, the synthesis of N bromine compounds is convenient, the structure is changeable, the arm length polymerization degree of the N-arm polystyrene containing the bromine end group can be accurately adjusted, and the method is a novel convenient and efficient crosslinked polystyrene synthesis method.

Description

technical field [0001] The invention relates to the field of preparation of cross-linked polystyrene, in particular to a method for preparing cross-linked polystyrene with evenly distributed branch points that can be decomposed and cross-linked. Background technique [0002] Condensation polymerization of polyfunctional monomers or copolymerization of vinyl monomers with a small amount of divinyl monomers can obtain crosslinked polymers. Compared with linear polymers, cross-linked polymers have a three-dimensional network structure, and their mechanical properties, thermal stability, wear resistance, solvent resistance and creep resistance are significantly different. It has important applications in the fields of drug release and controlled release of drugs. [0003] The structure of a cross-linked polymer has an important influence on its properties. The description of the cross-linking structure mainly includes the degree of cross-linking (or cross-linking density), the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F112/08C08F8/18
Inventor 王齐李承霖
Owner ZHEJIANG UNIV
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