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Synthesis of novel chain transfer agent with thermal initiation function

A chain transfer agent, thermally induced technology, applied in the direction of organic chemistry, etc., can solve the problems of reducing the polymerization rate, retardation effect, etc., to achieve the effect of reducing the amount of use and simplifying the implementation process

Active Publication Date: 2013-12-18
JIANGSU XUETAI PRINTING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It is important to note that the use of dithioesters, especially dithiobenzoates, has a severe retardation effect, which can greatly reduce the rate of polymerization

Method used

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  • Synthesis of novel chain transfer agent with thermal initiation function
  • Synthesis of novel chain transfer agent with thermal initiation function
  • Synthesis of novel chain transfer agent with thermal initiation function

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Step 1) Synthesis of trithioester S-n-dodecyl-S′-(2-isobutyryl) trithiocarbonate (X5) with carboxyl group: add in a 250 mL round bottom flask n-Dodecanethiol (37.3 g, 0.184 mol), acetone (107 g, 1.84 mol), Aliquat 336 (2.99 g, 7.37 mol), at 10 o Mix and stir evenly at C, add sodium hydroxide solution (50 wt %) (15.5 g, 0.193 mol) dropwise, at 10 o Stir for 30 min at C, CS 2 A mixed solution of (14.0 g, 0.18 mol) and acetone (18.6 g, 0.32 mol) was added dropwise for 20 min and stirred for 10 min. Chloroform (32.8 g, 0.28 mol) was added in one portion, followed by sodium hydroxide solution (50 wt %) (73.7 g, 0.922 mol) dropwise. The mixture was stirred overnight. Stop the reaction, add 300 mL of deionized water to the three-necked flask, and continue to drop HCl solution to pH ≈ 2. The solid part obtained by suction filtration was dissolved in isopropanol (300 mL) under vigorous stirring, and the insoluble part was removed. The filtrate was rotary evaporated and recry...

Embodiment 2

[0036] Example 2: Initiated by bis-[S-n-dodecyl-S'-(2-isobutyryl-4,4'-azocyanopentyl ester)]trithiocarbonate (X6) Agents and chain transfer agents to regulate the polymerization of various monomers

[0037] The bulk polymerization behavior of styrene (St), methyl acrylate (MA) and N-isopropylacrylamide (NIPAM) in RAFT was investigated using X6 as both initiator and chain transfer agent. The aggregation results are shown in Table 1. The results show that X6 has very good controllability to St, MA and NIPAM, the theoretical molecular weight of the polymer is consistent with the GPC molecular weight, and the molecular weight distribution of the polymer is narrow ( M w / M n < 1.16).

[0038] Numbering Initial molar ratio of monomer to regulating reagent X6 Reaction time (h) Conversion rates(%) Theoretical Number Average Molecule (g / mol) Measured number average molecular weight (g / mol ) molecular weight distribution index 1 [St]0:[X6]0=200:1 24 ...

Embodiment 3

[0041] Example 3: Using X6 as initiator and chain transfer agent, research on the polymerization behavior of St at different temperatures and different ratios

[0042] According to the polymerization results of Example 2, taking the St monomer as the research object, its polymerization behavior was investigated in detail.

[0043] Firstly, the polymerization behavior of the polymerization system with St was investigated at different temperatures using X6 as initiator and chain transfer agent at the same time. at 60 o C. 70 o C.90 o At C, the RAFT bulk polymerization and solution polymerization of St were done, and the polymerization results are shown in Table 2, Table 3, and Table 4. It can be seen from the table that under the three temperatures, X6 has a good controllability to St, but with the increase of reaction temperature, the polymerization speed is accelerated, especially at 90 o C, within 3 h, the conversion rate of the polymer can reach 85%. m w / M n There is...

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Abstract

The invention discloses synthesis of a novel chain transfer agent with a thermal initiation function. The synthesis comprises the following steps: firstly performing an esterification reaction on a carboxyl-containing trithio ester S-n-dodecyl-S'-(2-isobutyric acid group)trithiocarbonate and a hydroxyl-containing azo initiator 4,4-azobiscyano pentanol to synthesize bis-[S-n-dodecyl-S'-(2-isobutyric acid group-4,4'-azocyanoamyl ester]trithiocarbonate; and then inspecting the RAFT (reversible addition-fragmentation chain transfer) bulk polymerization behaviors of the monomers such as styrene, methyl acrylate, N-isopropylacrylamide and the like by taking the bis-[S-n-dodecyl-S'-(2-isobutyric acid group-4,4'-azocyanoamyl ester]trithiocarbonate as an initiator and a chain transfer agent. According to the synthesis disclosed by the invention, the initiator structure is introduced into the RAFT reagent structure to prepare a chain transfer agent with an initiation function, and the living radical polymerization of the monomers such as styrene and the like can be successfully implemented.

Description

technical field [0001] The present invention relates to the synthesis of a multifunctional regulating agent, in particular to the synthesis of a novel chain transfer agent with thermal initiation function. Background technique [0002] In 1998, Rizzardo et al. found that dithioesters can be used to obtain polymers with well-controlled molecular weight distribution, reversible addition-fragmentation chain transfer polymerization, that is, RAFT method, thus introducing "living" / controllable free radical polymerization, And it has become a method that has been studied more in recent years. The biggest advantage of RAFT polymerization is that it is applicable to a wide range of monomers. In addition to common monomers such as styrene and (meth)acrylates, it is also suitable for functional monomers such as hydroxyethyl methacrylate and sodium p-vinylbenzenesulfonate. Therefore, RAFT polymerization is very beneficial to the polymerization reaction of ethylenic monomers containing...

Claims

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Application Information

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IPC IPC(8): C08F2/38C08F4/04C08F12/08C08F20/14C08F20/54C07C329/00
Inventor 朱健吴英窦和琴张伟张正彪朱秀林
Owner JIANGSU XUETAI PRINTING
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