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Synthesis of novel chain transfer agent with thermal initiation function

A technology of chain transfer agent and thermal initiation, which is applied in the direction of organic chemistry, can solve problems such as retardation effect, reduce polymerization rate, etc., achieve the effect of reducing usage and simplifying the implementation process

Active Publication Date: 2015-07-01
JIANGSU XUETAI PRINTING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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] Table 1 GPC measurement results of polymerization of various monomers under the action of X6

[0039] Numbering Initial molar ratio of monomer to regulating reagent X6 Reaction time (h) Conversion rates(%) Theoretical Number Average Molecule (g / mol) Measured number a...

Embodiment 3

[0042] Example 3: Using X6 as initiator and chain transfer agent, research on the polymerization behavior of St at different temperatures and different ratios

[0043] According to the polymerization results of Example 2, taking the St monomer as the research object, its polymerization behavior was investigated in detail.

[0044] 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 the synthesis of a new type of chain transfer agent containing thermal initiation function. Bis-[S-n-dodecyl-S'-(2-isobutyric acid -4,4'-azocyanopentyl ester)] trithiocarbonate, followed by bis-[S-n-dodecyl-S'-(2-isobutyryl-4,4'- Azocyanopentyl ester)] trithiocarbonate as initiator and chain transfer agent for reversible addition-fragmentation chain transfer (RAFT) of monomers such as styrene, methyl acrylate, and N-isopropylacrylamide Aggregation behavior was examined. The invention introduces the initiator structure into the RAFT reagent structure, prepares the chain transfer reagent with initiating function, and can successfully carry out living free radical polymerization of monomers such as styrene.

Description

Technical field [0001] The invention involves a synthesis of a multifunctional regulatory reagent, which specifically involves a new type of chain transfer agent containing thermal function. Background technique [0002] In 1998, Rizzardo and others found that the use of sulfur ester to obtain a polymer with a good molecular weight distribution control, reversible bonus-fracture chain transfer aggregation, that is, Raft method, which introduced "activity" / controllable free radical polymerization.And it has become a way to study more in recent years.The biggest advantage of RAFT aggregation is the wide range of monomers. In addition to common monomers, (methyl) acrylate, it is also applicable to functional single such as methyl acrylic hydroxyl ethyl, sodium to ethylene,The body, so the RAFT aggregation is very conducive to the polymerization reactions of a special functional group (such as carboxyl, hydroxyl, dilate, etc.).Raft aggregation molecular weight distribution is narrow ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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