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Quaternary ammonium salt water-soluble trithiocarbonate RAFT (reversible addition-fragmentation chain transfer polymerization) reagent and preparation method thereof

A technology of trithiocarbonate and alkyl trithiocarboxylic acid, which is applied in the field of RAFT reagent synthesis, can solve problems such as the synthesis of water-based RAFT reagents and the like, and achieve the effects of widening the scope, simple preparation process and high water compatibility

Inactive Publication Date: 2018-08-07
陈晨特
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, the existing literature and patents rarely involve the synthesis of aqueous RAFT reagents

Method used

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  • Quaternary ammonium salt water-soluble trithiocarbonate RAFT (reversible addition-fragmentation chain transfer polymerization) reagent and preparation method thereof
  • Quaternary ammonium salt water-soluble trithiocarbonate RAFT (reversible addition-fragmentation chain transfer polymerization) reagent and preparation method thereof
  • Quaternary ammonium salt water-soluble trithiocarbonate RAFT (reversible addition-fragmentation chain transfer polymerization) reagent and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0022] A kind of preparation method of quaternary ammonium salt type water-soluble trithiocarbonate RAFT reagent comprises the steps:

[0023] (1) Synthesis of alkyl trithioformic anhydride: Add 6 parts of elemental sodium and 180 parts of toluene into the reactor and stir well, then keep the temperature at 5°C, and add 12 parts of n-hexylsulfur dropwise to the reactor Alcohol, after 30 minutes of dropwise addition, continue the reaction at 5°C for 0.5h to obtain a dispersion of sodium n-hexylmercaptide; cool the dispersion of sodium n-hexylmercaptide to 0°C, add 12 parts of carbon disulfide to it, and react fully for 3 hours to obtain an alkyl Sodium trithiocarbonate dispersion; then keep stirring, at 40°C, add 8g of solid iodine to the alkyl sodium trithiocarbonate dispersion, react for 3h, filter to remove the precipitate to obtain a yellow-brown filtrate; extract with sodium thiosulfate solution Unreacted elemental iodine in the filtrate, then add anhydrous magnesium chlor...

Embodiment 2

[0026] A kind of preparation method of quaternary ammonium salt type water-soluble trithiocarbonate RAFT reagent comprises the steps:

[0027] (1) Synthesis of alkyl trithioformic anhydride: Add 10 parts of sodium hydride and 160 parts of diethyl ether into the reactor and stir well, then keep the temperature at 10°C, and add 20 parts of n-pentyl Mercaptan, after 15 minutes of dropwise addition, continue the reaction at 10°C for 0.5h to obtain a dispersion of sodium n-pentylmercaptide; cool the dispersion of sodium n-pentylmercaptide to -5°C, add 8 parts of carbon disulfide to it, and fully react for 1 hour , to obtain a dispersion of alkyl sodium trithiocarbonate; then keep stirring, at 20°C, add 4g of solid iodine to the dispersion of alkyl sodium trithiocarbonate, react for 1h, filter and remove the precipitate to obtain a yellow-brown filtrate; Extract unreacted elemental iodine in the filtrate with sodium sulfate solution, then add anhydrous magnesium chloride to it and d...

Embodiment 3

[0030] A kind of preparation method of quaternary ammonium salt type water-soluble trithiocarbonate RAFT reagent comprises the steps:

[0031] (1) Synthesis of alkyl trithioformic anhydride: Add 9 parts of sodium hydride and 130 parts of n-butyl ether into the reactor and stir well, then keep the temperature at 0°C, and add 10 parts of n-butyl ether dropwise to the reactor. Butyl mercaptan, after 15 minutes of dropwise addition, continue the reaction at 0°C for 0.5h to obtain a dispersion of sodium n-butylmercaptide; cool the dispersion of sodium n-butylmercaptide to -2°C, add 9 parts of carbon disulfide to it, and fully React for 2 hours to obtain a dispersion of alkyl sodium trithiocarbonate; then keep stirring at 35°C, add 6.5 g of solid iodine to the dispersion of alkyl sodium trithiocarbonate, react for 2.5 hours, filter to remove the precipitate to obtain a yellow-brown filtrate ; Extract the unreacted elemental iodine in the filtrate with sodium thiosulfate solution, th...

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Abstract

The invention relates to a quaternary ammonium salt water-soluble trithiocarbonate RAFT (reversible addition-fragmentation chain transfer polymerization) reagent. The structure of the quaternary ammonium salt water-soluble trithiocarbonate RAFT reagent is as shown in an attached figure (n: 1-9, m: 3-6, R is CH3, CH2CH3, CH2CH2CH3 or CH2CH2CH2CH3, X is Br or I). The synthesis principle of the reagent includes that alkyl sodium mercaptan is firstly synthesized and reacts with carbon disulfide to obtain alkyl sodium trithiocarbonate, the alkyl sodium trithiocarbonate is coupled into alkyl trithio-formic anhydride, and finally, the alkyl trithio-formic anhydride sequentially reacts with tertiary amine and halogenated hydrocarbon in azo functional groups to prepare the RAFT reagent. The RAFT reagent has high water solubility and a wide application prospect and is suitable for water solution free radical polymerization and emulsion polymerization, the synthesized polymer is large in molecular weight, and dispersion coefficient is smaller than 1.2.

Description

technical field [0001] The invention relates to a quaternary ammonium salt type water-soluble trithiocarbonate RAFT reagent and a preparation method thereof, belonging to the field of RAFT reagent synthesis. technical background [0002] RAFT is the abbreviation of Reversible Addition-Fragmentation Chain Transfer Polymerization (Reversible Addition-Fragmentation Chain Transfer Polymerization), which is a kind of living / controllable radical polymerization (CRP). [0003] In RAFT reactions, dithioester derivatives are usually added as chain transfer reagents. In the polymerization, it forms a dormant intermediate with the free radicals of the growing chain, which limits the irreversible double-radical termination side reaction between the free radicals of the growing chain, so that the polymerization reaction can be effectively controlled. This dormant intermediate can be cleaved by itself, and new active free radicals are released from the corresponding sulfur atoms, and com...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F2/38C07C329/00C08F120/06
CPCC07C329/00C08F2/38C08F120/06C08F2438/03
Inventor 陈晨特
Owner 陈晨特
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