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Method for preparing crosslinked polystyrene or crosslinked copolymer

A technology of cross-linked polystyrene and cross-linked copolymers, which is applied in the field of cross-linked polymer preparation to achieve the effects of simple synthesis conditions, convenient synthesis, and high reactivity

Active Publication Date: 2016-05-25
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 crosslinked polystyrene or crosslinked copolymer
  • Method for preparing crosslinked polystyrene or crosslinked copolymer
  • Method for preparing crosslinked polystyrene or crosslinked copolymer

Examples

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Embodiment 1

[0040] The synthesis of embodiment 1 polyamine ligand TPMA

[0041] 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

[0042] The synthesis of embodiment 2 polyamine ligand TPEN

[0043] 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

[0044] Synthesis of embodiment 3 small molecule polybrominated compound 3a

[0045] 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) in DCM (50 mL) was dropped into a three-necked flask, and after 1 hour, a white precipitate appeared, and the temperature was raised to room temperature (25° C.), and stirred overnight for 18 hours. 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...

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Abstract

The invention relates to the field of crosslinked polymer preparation and aims at providing a method for preparing crosslinked polystyrene or crosslinked copolymer. The method comprises the steps of taking micromolecule polybromide, styrene monomer, polyamine ligand and solvent for a reaction and deoxidation, and adding copper powder under protection of nitrogen; conducting a reaction to obtain the crosslinked polystyrene with branch point distribution measurable; or treating dobby polyoxyethylene brominated with the end group or other macromolecule polybromide as initiator instead of micromolecule polybromide, so that crosslinked copolymer with branch point distribution measurable is obtained under the same reaction condition. The method is simple in synthesis condition, and polybromide is convenient to synthesize and variable in structure; a divinyl monomer does not needed to be added as a cross-linking agent; a product is high in reactivity, the method is simple and convenient, and the preparation condition is mild; degradable branch points are available, and the crosslinked polystyrene different in function can be prepared by changing the varieties of the macromolecule polybromide. High potential application value is achieved.

Description

technical field [0001] The invention relates to the field of cross-linked polymer preparation, in particular to a method for preparing cross-linked polystyrene or cross-linked copolymer in one step. 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 distribution of cross-linking points and the c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F112/08C08F4/54
CPCC08F4/54C08F112/08
Inventor 王齐李承霖
Owner ZHEJIANG UNIV
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