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A kind of living free radical polymerization method that is used in combination with aromatic cyclic thio (oxo) thioketone and its derivatives and free radical initiator

A polymerization method and free radical technology, applied in the direction of organic chemistry, can solve the problems of insignificant molecular weight growth, huge molecular weight distribution, high initiating activity, etc., and achieve the effect of wide application range

Active Publication Date: 2018-01-12
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because what this system uses is not a thione with a ring-shaped aromatic structure, but a thione that is connected to both sides of the carbon atom of the carbon-sulfur double bond (C=S) that plays a major regulatory role by two conjugated groups, The initiation activity of the carbon atom is high, and at the same time, the coupling ability with the chain radical is small, and finally the product obtained by the above method has no obvious increase in molecular weight, and the molecular weight distribution is very large
Can not play a role in effective regulation of molecular weight and molecular weight distribution

Method used

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  • A kind of living free radical polymerization method that is used in combination with aromatic cyclic thio (oxo) thioketone and its derivatives and free radical initiator
  • A kind of living free radical polymerization method that is used in combination with aromatic cyclic thio (oxo) thioketone and its derivatives and free radical initiator
  • A kind of living free radical polymerization method that is used in combination with aromatic cyclic thio (oxo) thioketone and its derivatives and free radical initiator

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Example 1: Thiathione regulates MMA solution polymerization at different reaction temperatures.

[0046] In a 100ml single-necked bottle, add 0.0500g of thiathione, 0.0164g of AIBN, 5.0000g of MMA, and 15g of toluene. After sealing, freezing and thawing and degassing three times, react at 70 degrees and 80 degrees respectively for 24 hours. Take out the samples regularly and quickly place them in liquid nitrogen to quench them. After vacuum drying, the conversion rate of the monomers increases linearly with the reaction time as measured by gravimetric method; Large, the dispersion coefficient is basically below 1.8. The obtained living free radical polymer can be used as a macroinitiator to continue to initiate block copolymerization of other monomers.

[0047] The results of the 70 degree experiment are shown in Table 1.

[0048] time (hours)

Conversion rates(%)

molecular weight

polydispersity coefficient

1

27.2

41400

1.78

...

Embodiment 2

[0051] Example 2: Thiathione regulates MMA solution polymerization at different MMA concentrations.

[0052] In a 100ml single-necked bottle, add thiathione, AIBN, MMA and toluene. Add thiathione, AIBN, MMA and toluene, AIBN, thiothione mass are 0.0328g and 0.1000g respectively; MMA mass are 2.50g, 5.00g, 10.00g respectively. The total of MMA and toluene is 20.00g. Sealed, freeze-thawed and degassed three times, and reacted at 70 degrees for 24 hours. The samples were taken out regularly and quickly placed in liquid nitrogen to quench them. After vacuum drying, the monomer conversion rates of the two groups of experiments were measured by gravimetric method. The monomer conversion rate increased linearly with the reaction time; rate increases.

[0053] MMA concentration is 12.5% ​​experimental results are shown in Table 3.

[0054] time (hours)

Conversion rates(%)

molecular weight

polydispersity coefficient

[0055] 1

8.2

16,300

...

Embodiment 3

[0060] Example 3: 70-degree thiathione regulates BA solution polymerization

[0061] In a 100ml single-necked bottle, 0.0500g of thiothione, 0.0164g of AIBN, 5.00g of BA, and 15.00g of toluene. Sealed, freeze-thawed and degassed three times, and reacted at 70 degrees for 24 hours. Take out the samples regularly and quickly place them in liquid nitrogen to quench them. After vacuum drying, the monomer conversion rate increases with the prolongation of the reaction time as measured by gravimetric method; the molecular weight increases with the increase of the monomer conversion rate as observed by GPC , The dispersion coefficient is around 1.8. The obtained active polymer can be used as a macroinitiator to initiate block copolymerization of other monomers.

[0062] The experimental results are shown in Table 6.

[0063] time (hours)

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Abstract

Disclosed in the present invention is a living free radical polymerization based on combined use of aromatic cyclic thia-(oxa-) thioketone, derivatives of the aromatic cyclic thia-(oxa-) thioketone and free radical initiators. According to the method, the aromatic cyclic thioketone (C=S-Ph2(X)) and derivatives of the aromatic cyclic thioketone are used as initiation control agents, two benzene rings are connected, and then controllable / living free radical polymerization is implemented on vinyl monomers, X being C, N, O and S. The method is characterized in that C＝S-Ph2(X) and derivatives of the C＝S-Ph2(X) are used together with traditional free radical initiators such as AIBN, and polymers having controllable molecular weight and distribution and having dormancy groups at each one end can be obtained under the heating condition; and the obtained polymers can also be used as macroinitiator for initiating other monomers to prepare a segmented copolymer. The polymerization method used in the present invention has a simple operation process, monomers have wide application ranges and can be used in polymerization methods such as thermal polymerization methods of bodies, solutions, emulsions, suspensions and the like, and a good basis is created for industrial application of living free radical polymerization reactions.

Description

technical field [0001] The present invention relates to a method for preparing active radical polymers using a class of initiation control agents derived from X heterothione structures and derivatives thereof, and a method for preparing block copolymers using the active radical polymers as macromolecular initiators . Background technique [0002] Polymer materials with controllable molecular weight and molecular weight distribution have a wide range of applications in the fields of polymer crystallography, self-assembly, synthesis and preparation of new materials, surface modification, and biomedicine. Therefore, the molecular weight and distribution can be prepared Controlled polymer materials have attracted great attention from science and industry. At present, there have been a lot of research work on living polymerization, including living anionic polymerization, living cationic polymerization, living coordination polymerization, living ring-opening polymerization and l...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F120/14C08F120/18C08F120/32C08F112/08C08F2/02C08F293/00C07D335/14
CPCC07D335/14C08F2/02C08F112/08C08F120/14C08F120/18C08F120/32C08F293/00
Inventor 杨万泰闫煦王力
Owner BEIJING UNIV OF CHEM TECH
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