Method for synthesizing poly(sodium-styrenesulfonate) with terpyridyl ruthenium initiator

A technology of sodium polystyrene sulfonate and ruthenium terpyridine, which is applied in the field of synthesizing sodium polystyrene sulfonate, controllable PSS, and uniform molecular weight, which can solve the development limitation of photo-induced RAFT polymerization and the narrow wavelength range of photo-polymerization , low initiator initiation efficiency and other issues, to achieve the effect of good product quality, strong stability and high preparation efficiency

Inactive Publication Date: 2016-08-24
QINGDAO UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the development of photoinitiated RAFT polymerization has been limited due to the narrow wavelength range that can initiate photopolymerization, the low efficiency of initiators, and the environmental safety caused by the pollution of initiators to the environment.

Method used

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  • Method for synthesizing poly(sodium-styrenesulfonate) with terpyridyl ruthenium initiator
  • Method for synthesizing poly(sodium-styrenesulfonate) with terpyridyl ruthenium initiator
  • Method for synthesizing poly(sodium-styrenesulfonate) with terpyridyl ruthenium initiator

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 1. Using ruthenium terpyridine as a photoinitiator to initiate RAFT polymerization to prepare polymer PSS:

[0029] (1) Put 40mg RAFT reagent (4-cyano-4-ethyltrithiovaleric acid, CETP), 4g sodium p-styrenesulfonate and 5mg ruthenium terpyridyl in a 50mL volumetric flask with 8mL water and 9mL di Oxycycline was dissolved to obtain a reagent for subsequent use;

[0030] (2) feed nitrogen into the volumetric flask equipped with reagent in step (1) to remove oxygen for 70 minutes;

[0031] (3) irradiating the volumetric flask after deoxygenation in step (2) for 24h under the blue light of 200W;

[0032] (4) dialyze the product obtained in step (3) in ultrapure water for 4 days, then put it into a vacuum box and dry it to obtain the polymer PSS;

[0033] 2. Pyrene functionalization of RAFT reagent (CETP):

[0034] (1) Dissolve 0.5g pyrenemethanol, 0.73g CETP, 0.6383g dicyclohexylcarbodiimide (DCC) and 0.0378g 4-dimethylaminopyridine (DMAP) in 10mL tetrahydrofuran (THF) re...

Embodiment 2

[0043] In this example, the synthetic PCETP and PSS were characterized by NMR. figure 2 A is the NMR characterization of PECTP, figure 2 B is the NMR characterization of PSS. Through the analysis of each peak position on the NMR spectrum, it is proved that PCETP and PSS were successfully synthesized in this embodiment.

Embodiment 3

[0045] The present embodiment has characterized the molecular weight, dispersity and conversion rate of PSS, as image 3 Shown in A, the reaction time increases, and the conversion rate of polymer PSS is higher and higher, reaches 79% in 24 hours; As image 3 As shown in B, the difference between the molecular weight of the polymer measured by gel permeation chromatography (GPC) and the theoretical molecular weight is within 2%, and the molecular weight distribution of PSS is very narrow, less than 1.28.

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Abstract

The invention belongs to the technical field of chemical synthesis and relates to a method for synthesizing PSS (poly(sodium-styrenesulfonate)) with uniform molecular weight and controllability by polymerization of reversible addition fragmentation chain transfer (RAFT) based on terpyridyl ruthenium serving as a photoinitiator. The method comprises: preparing PSS mainly from 4-cyano-4-ethyltrithiopentanoic acid, sodium p-styrenesulfonate and terpyridyl ruthenium, using pyrenemethanol, 4-cyano-4-ethyltrithiopentanoic acid (CETP), dicyclohexylcarbodiimide (DCC), 4-dimethylaminopyridine (DMAP) and tetrahydrofuran (THF) to prepare a functionalized RAFT reagent (4-cyano-4-ethyltrithiopentanoic acid CETP), and the using the functionalized RAFT reagent (4-cyano-4-ethyltrithiopentanoic acid CETP) to prepare PSS. The preparation process is simple, preparation efficiency is high, product quality is good, product stability is high, and a product is friendly to application environments.

Description

Technical field: [0001] The invention belongs to the technical field of chemical synthesis, and relates to a method for synthesizing polystyrene sodium sulfonate (PSS), in particular to a method based on ruthenium terpyridine as a photoinitiator, which is polymerized by reversible addition-fragmentation chain transfer (RAFT). A method for synthesizing PSS with uniform and controllable molecular weight under the irradiation of blue light at room temperature. Background technique: [0002] PSS is an excellent anionic polyelectrolyte, and PSS solution is a water-soluble polymer with unique functions, which is reused in various fields of industry, such as reactive emulsifiers, water-soluble polymers (coagulant , dispersant, container cleaning agent, cosmetics, etc.), water treatment agent (dispersant, flocculant), sulfur exchange resin (membrane), photo agent (membrane), semiconductor, image film, heat conduction products, etc. In the above-mentioned fields of application, vari...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F112/14C08F2/48C08F2/38
CPCC08F112/14C08F2500/03C08F2/48C08F2/38
Inventor 刘敬权许元红陈涛
Owner QINGDAO UNIV
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