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Preparation method for efficient chain transfer agent trithiocarbonate used for RAFT (reversible addition-fragmentation chain transfer) polymerization

A technology of chain transfer polymerization and addition-fragmentation, which is applied in organic chemistry and other fields, can solve the problems of complex preparation process, complicated post-processing, and difficulty in long-term storage, and achieve the effects of high product purity, convenient purification, and simple synthesis method

Inactive Publication Date: 2012-09-26
TONGJI UNIV
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  • Summary
  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] Although the above-mentioned water-soluble dithioesters have a certain chain transfer effect in RAFT polymerization, the preparation process of dithioesters is complicated, and some toxic reagents are often used, and the post-treatment is complicated, the product is unstable, and it is difficult to store for a long time

Method used

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  • Preparation method for efficient chain transfer agent trithiocarbonate used for RAFT (reversible addition-fragmentation chain transfer) polymerization
  • Preparation method for efficient chain transfer agent trithiocarbonate used for RAFT (reversible addition-fragmentation chain transfer) polymerization
  • Preparation method for efficient chain transfer agent trithiocarbonate used for RAFT (reversible addition-fragmentation chain transfer) polymerization

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Experimental program
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Effect test

Embodiment 1

[0026] Add 2 g of potassium phosphate (K 3 PO 4 ) and 50mL of acetone, followed by 2g of carbon disulfide (CS 2 ) into a round-bottomed flask through a syringe, and stirred for 1 h; 2 g of dodecanethiol was added into a round-bottomed flask, and stirred for 1 h; finally, 1.5 g of 2-bromoisobutyric acid was added, and the reaction was carried out for 13 h. After the reaction, the solvent acetone was removed by distillation under reduced pressure, and the bright yellow trithioester C was obtained through dissolution, extraction and washing. 17 h 32 o 2 S 3 .

[0027] figure 1 Molecular formula for trithioester.

Embodiment 2

[0029] Add 15g potassium phosphate (K 3 PO 4 ) and 200mL of acetone, followed by 10g of carbon disulfide (CS 2 ) into a round-bottomed flask through a syringe, and stirred for 3 hours; 10 g of dodecanethiol was added into a round-bottomed flask, and stirred for 3 hours; finally, 7.5 g of 2-bromoisobutyric acid was added, and the reaction was carried out for 24 hours. The solvent after the reaction was removed by distillation under reduced pressure, and the bright yellow trithioester C was obtained by dissolving, extracting and washing. 17 h 32 o 2 S 3 .

Embodiment 3

[0031] Add 20g potassium phosphate (K 3 PO 4 ) and 500mL of acetone, followed by 20g of carbon disulfide (CS 2 ) into a round-bottomed flask through a syringe, and stirred for 4 hours; 20g of dodecanethiol was added into a round-bottomed flask, and stirred for 3 hours; finally, 15g of 2-bromoisobutyric acid was added, and the reaction was carried out for 24 hours. The solvent after the reaction was removed by distillation under reduced pressure, and the bright yellow trithioester C was obtained by dissolving, extracting and washing. 17 h 32 o 2 S 3 .

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Abstract

The invention belongs to the field of polymer nano biological medicinal materials, particularly relates to a preparation method for efficient chain transfer agent trithiocarbonate used for RAFT polymerization. The method is characterized in that the chemical formula of the trithiocarbonate is C17H32O2S3, and comprises the following steps: adding potassium phosphate, a solvent and carbon bisulfide into a round-bottom flask for reaction 1-3 hours; adding do-decyl mercaptans to conduct addition reaction for 1-3 hours; and finally adding 2-bromine isobutyric acid to conduct esterification reaction for 13-24 hours. The brilliant orange trithiocarbonate can be obtained from the reacted solvent subjected to procedures of reduced pressure distillation for removal, dissolution, extraction, and washing, wherein the mass ratio of the potassium phosphate to the carbon bisulfide is 1:(1-3), as well as the mass ratio of the do-decyl mercaptans to the carbon bisulfide, and the mass ratio of the 2-bromine isobutyric acid to the carbon bisulfide are also 1: (1-3). According to the method provided by the invention, the synthesizing is simple, the purification is convenient, and the stability of the product is good. Moreover, the RAFT polymerization has an efficient chain transfer effect. Therefore, the method is favorable for advancing the RAFT large-scale industrial production, and has an extensive application prospect.

Description

technical field [0001] The invention belongs to the field of macromolecule nano biomedical materials, and in particular relates to a preparation method of a high-efficiency chain transfer agent trithioester for reversible addition-fragmentation chain transfer polymerization. Background technique [0002] The concept of living polymerization (living polymerization) was proposed by Szwarc in 1956, that is, a polymerization reaction in which there is no termination, no transfer, and the initiation rate is much greater than the growth rate. Since there is no chain transfer, the number of polymer chains remains constant during polymerization; there is no chain termination. Until the monomer in the system is consumed and the polymerization reaction stops, the polymer chain still maintains active groups. Polymerization can continue as soon as new monomer is added. So Szwarc called this polymerization method "Living Polymerization". [0003] Australian Chiefari, Rizzardo et al. f...

Claims

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Application Information

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IPC IPC(8): C07C329/00C08F2/38
Inventor 杜建忠路航
Owner TONGJI UNIV
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