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Preparation method of organic silicon-based RAFT (reversible addition-fragmentation chain transfer) reagent

An organosilicon and reagent technology, applied in the field of preparation of organosilicon-based RAFT reagents, can solve the problems of low introduction of organosilicon, poor dispersibility, volatile organic pollution, etc. The effect of decomposition

Pending Publication Date: 2022-04-05
NANJING FORESTRY UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to provide a preparation method of organosilicon-based RAFT reagents, to develop a method that can effectively solve the problem of relatively low amount of organosilicon introduced in the synthesis of coatings, defoamers and surface sizing agents in RAFT polymerization, and the lack of organosilicon monotony Difficult to polymerize, silane active groups are prone to self-crosslinking, volatile organic pollution, poor defoaming performance, poor dispersion, poor water resistance of the sizing surface, etc., providing a more effective method for the preparation of silicone modified acrylic resin method

Method used

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  • Preparation method of organic silicon-based RAFT (reversible addition-fragmentation chain transfer) reagent
  • Preparation method of organic silicon-based RAFT (reversible addition-fragmentation chain transfer) reagent
  • Preparation method of organic silicon-based RAFT (reversible addition-fragmentation chain transfer) reagent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] Add 7.2g of mercaptopropyldimethoxymethylsilane, 40g of dimethyl sulfoxide, and 6.2g of triethylamine into the reaction kettle, stir for 20 minutes at normal temperature and pressure at 400rpm, then add 8.2g of carbon disulfide, and Electric substitution reaction, the reaction time is 4 hours; after the reaction, add 6.5g of methyl dibromoisobutyrate, through the electrophilic substitution reaction for 14 hours, and then wash with water to remove the solvent under reduced pressure to obtain the RAFT reagent. Finally, add 1g of RAFT reagent, 9g of diethoxydimethoxysilane, 0.46g of hexamethyldisiloxane, 2g of concentrated hydrochloric acid, 6g of deionized water, and 20g of n-hexane into the reaction kettle, at 75°C and 400rpm After reacting for 6 hours, the acid water was removed by chromatography, and the solvent was distilled off under reduced pressure to obtain an organosilicon-based RAFT reagent.

Embodiment 2

[0065] Add 7.2g of mercaptopropyldimethoxymethylsilane, 40g of dimethyl sulfoxide, and 6.2g of triethylamine into the reaction kettle, stir for 20 minutes at normal temperature and pressure at 400rpm, then add 8.2g of carbon disulfide, and Electric substitution reaction, the reaction time is 4 hours; after the reaction, add 6.5g of methyl dibromoisobutyrate, through the electrophilic substitution reaction for 14 hours, and then wash with water to remove the solvent under reduced pressure to obtain the RAFT reagent. Finally, 1.185g of RAFT reagent, 15.81g of diethoxydimethoxysilane, 0.54g of hexamethyldisiloxane, 2g of concentrated hydrochloric acid, 6g of deionized water, and 25g of n-hexane were added to the reaction kettle, at 70°C and 400rpm The reaction was carried out under the conditions for 5 hours, the acid water was removed by chromatography, and the solvent was distilled off under reduced pressure to obtain an organosilicon-based RAFT reagent.

Embodiment 3

[0067] Add 7.2g of mercaptopropyldimethoxymethylsilane, 40g of dimethyl sulfoxide, and 6.2g of triethylamine into the reaction kettle, stir for 20 minutes at normal temperature and pressure at 400rpm, then add 8.2g of carbon disulfide, and Electric substitution reaction, the reaction time is 4 hours; after the reaction, add 6.5g of methyl dibromoisobutyrate, through the electrophilic substitution reaction for 14 hours, and then wash with water to remove the solvent under reduced pressure to obtain the RAFT reagent. Finally, 2.37g of RAFT reagent, 11.85g of diethoxydimethoxysilane, 1.08g of hexamethyldisiloxane, 2g of concentrated hydrochloric acid, 6g of deionized water, and 25g of n-hexane were added to the reaction kettle, at 70°C and 400rpm The reaction was carried out under the conditions for 5 hours, the acid water was removed by chromatography, and the solvent was distilled off under reduced pressure to obtain an organosilicon-based RAFT reagent.

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Abstract

The invention discloses a preparation method of an organic silicon-based RAFT (reversible addition-fragmentation chain transfer) reagent, which comprises the following steps: by taking mercaptopropyl dimethoxy methylsilane, carbon disulfide and methyl dibromoisobutyrate as raw materials, carrying out electrophilic substitution reaction under the action of a high-polarity solvent and an amine organic base catalyst at normal temperature and normal pressure, and then removing the high-polarity solvent through washing and reduced pressure distillation to prepare the RAFT reagent; the preparation method comprises the following steps: by taking an RAFT reagent, a silane monomer and hexamethyldisiloxane as raw materials, under the action of a low-polarity solvent and an acid or alkali catalyst, carrying out silane hydrolysis reaction at the temperature of 40-90 DEG C and normal pressure, and finally removing acid water and the low-polarity solvent to prepare the organic silicon-based RAFT reagent. The organosilicon modified acrylate anti-doodling emulsion prepared by using the organosilicon-based RAFT reagent not only has the characteristics of stain resistance, scrubbing resistance, solvent resistance and the like, but also has the characteristics of excellent heat resistance, water resistance, oxidation resistance and the like, and can be widely applied to the fields of coatings, defoaming agents, surface sizing agents and the like.

Description

technical field [0001] The invention relates to a preparation method of an organosilicon-based RAFT reagent, belonging to the field of fine chemical chemicals. Background technique [0002] Since the concept of living polymerization was proposed in the 1960s, living polymerization has made continuous progress, and RAFT polymerization is widely used in emulsions because of its mild reaction conditions, wide range of monomers, and the ability to control molecular structure and molecular weight. , in different polymerization systems such as solution and suspension, and thus has received extensive attention from the industry. The main varieties of RAFT reagents include dithioesters, trithiocarbonates, dithiocarbamates and xanthates. At present, the RAFT reagents of dithioester, trithiocarbonate, dithiocarbamate and xanthate commonly used in the domestic market are poor in stability, poor in heat resistance, poor in oxidation resistance, easy to hydrolyze, and difficult to intro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/392
Inventor 季永新余奇伟吕正伟陈永康
Owner NANJING FORESTRY UNIV
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