A kind of preparation method of polyglycolide

A technology of polyglycolide and glycolide, which is applied in the field of aminoanilinolithium compounds and its preparation, can solve the problems of rapid development of polymer materials, aggravated pollution, difficult degradation of polymer materials, etc., and achieve catalyst structure Variety of effects with less metal residue and controllable molecular weight

Inactive Publication Date: 2016-06-22
UNIV OF JINAN
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Problems solved by technology

[0002] The birth of polymer materials based on petroleum has changed our lives. A variety of high-performance polymer materials have been ubiquitous in every corner of our daily life, bringing unprecedented convenience to our lives, but What is worrying is that under the background of increasing global oil tension, the rapid development of polymer materials dependent on petroleum raw materials is greatly restricted
Moreover, high molecular polymer materials are difficult to degrade, and a large amount of high molecular polymer material waste has accumulated in real life for a long time, and the pollution to the human living environment has gradually increased.

Method used

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  • A kind of preparation method of polyglycolide
  • A kind of preparation method of polyglycolide
  • A kind of preparation method of polyglycolide

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] The structural formula of the ligand used is the above formula (A), where Ar is 4-methylphenyl, and the reaction process is as follows: under a nitrogen atmosphere, dissolve 0.51 g of the ligand in 10 mL of dry n-hexane, and add equimolar A certain amount of n-butyllithium was slowly raised to room temperature for 3 hours, filtered and washed with dry n-hexane, collected and dried to weigh 0.49g solid, yield 94%.

[0044] The NMR information of the obtained product is as follows. It can be seen from the NMR information that the lithium compound whose Ar is 4-methylphenyl was successfully synthesized.

[0045] 1 HNMR (400MHz, CDCl 3 ) δ 7.40(d, J =7.5Hz,2H,Ph- H ), 7.24–6.91 (m, 10H, Ph- H ),6.62(d, J =7.6Hz,2H,Ph- H ),4.40(s,4H,C H 2 N),2.72(s,12H,NC H 3 ),2.20(s,6H,C H 3 ).

[0046] 13 CNMR (100MHz, CDCl 3 ) δ152.45, 146.61, 134.27, 129.81, 128.23, 127.98, 126.66, 124.17, 116.34, 114.34, 48.86, 45.46, 20.40.

Embodiment 2

[0048] The structural formula of the ligand used is the above formula (A), where Ar is 2,6-dimethylphenyl, and the reaction process is as follows: under a nitrogen atmosphere, dissolve 0.47g of the ligand in 10mL of dry cyclohexane, and at 0°C Add 1.05 times the molar amount of n-butyllithium, slowly rise to room temperature and react for 6 hours, filter and wash the filter cake with dry n-hexane, collect and dry and weigh to obtain 0.46g solid, yield 95%.

[0049] The NMR information of the obtained product is as follows. It can be seen from the NMR information that the lithium compound whose Ar is 2,6-dimethylphenyl was successfully synthesized.

[0050] 1 HNMR (400MHz, CDCl 3 ) δ 7.42 (dd, J =6.2,1.3Hz,2H,Ph- H ),7.28-7.25(m,2H,Ph- H ),7.17(dd, J =7.0,1.0Hz,2H,Ph- H ),7.06(td, J =7.4,1.2Hz,2H),7.00(d, J =7.4Hz,4H),6.83(t, J =7.5Hz,2H),4.17(s,4H,NC H 2 Ph),2.73(s,12H,NC H 3 ),2.31(s,12H,PhC H 3 ).

[0051] 13 CNMR (100MHz, CDCl 3 ) δ 152.80, 146.54, 135...

Embodiment 3

[0053] The structural formula of the ligand used is the above formula (A), where Ar is 2,6-diethylphenyl, and the reaction process is as follows: under a nitrogen atmosphere, dissolve 0.34 g of the ligand in 5 mL of dry toluene, and add 1.1 times the molar amount of methyllithium was raised to room temperature and reacted for 1 hour, filtered and washed with dry n-hexane, collected, dried and weighed to obtain 0.32g, with a yield of 91%.

[0054] The crystal structure of the obtained product is shown in figure 1 As shown, the NMR information is as follows, it can be seen that the lithium compound whose Ar is 2,6-diethylphenyl was successfully synthesized.

[0055] 1 HNMR (400MHz, CDCl 3 ) δ 7.48–7.45 (m,2H,Ph- H ),7.29(dd, J =7.8,1.5Hz,2H,Ph- H ),7.19(dd, J =8.0,1.1Hz,2H,Ph- H ),7.13(d, J =7.9Hz,2H,Ph- H ),7.09(m,4H,Ph- H ),6.97(dd, J =8.1,6.9Hz,2H,Ph- H ),4.12(s,4H,NC H 2 Ph),2.73(s,12H,NC H 3 ),2.52(q, J =7.5Hz,8H,C H 2 CH 3 ),1.15(t, J =7.5Hz,12H,CH ...

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Abstract

The invention discloses a preparation method of polyglycolide, comprising the following steps: mixing a catalyst, an organic solvent, and glycolide, performing ring-opening polymerization reaction under the protection of anhydrous, oxygen-free and inert gas, and carrying out the reactant after the reaction Polyglycolide is processed; the catalyst is an aminoanilide lithium compound. The invention uses the aminoanilinolithium compound as a catalyst, has good reaction controllability, mild conditions, fast reaction rate, polymerization reaction can occur without adding an alcohol co-catalyst, high catalytic activity, and the molecular weight of the obtained polyglycolide is controllable , high yield, less metal residue. In addition, the polymerization reaction process of the present invention is simple, the usual solution polymerization method can be adopted, the molecular weight of the polymer can be regulated through the control of the polymerization reaction conditions, the selectivity is wide, and the molecular weight distribution of the obtained polymer is narrow, with excellent physical and chemical properties, Can meet the needs of the market.

Description

Technical field [0001] The present invention involves an amino anil anilinel lithium compound and its preparation method, and also involves the method of preparing polyethyl ester as a catalyst. Background technique [0002] The birth of polymer materials with oil as raw materials has changed our lives. A variety of high -performance polymer materials have generally existed in every corner of our daily life, bringing unprecedented convenience to our lives, but orderingIt is worried that in the context of the increasingly tense global oil, the rapid development of high molecular materials relying on oil raw materials has been greatly restricted.Moreover, the polymer polymerization materials are difficult to degrade, and a large amount of polymer polymerization materials have been accumulated in real life in real life.Traditional polymer materials face two major problems in the energy crisis and environmental pollution. It is a trend of the development of polymer aggregate material...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/06C08G63/83C07C211/65C07C209/00
Inventor 姚伟徐征和高爱红王昕张云苹朱广云
Owner UNIV OF JINAN
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