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A kind of preparation method of polycaprolactone

A technology of polycaprolactone and catalyst is applied in the field of preparing polycaprolactone, which can solve the problems of rapid development of polymer materials, difficult degradation of polymer materials, and increased pollution, and achieves diverse catalyst structure changes and controllable molecular weight. , the effect of less metal residue

Inactive Publication Date: 2016-06-29
UNIV OF JINAN
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  • Abstract
  • Description
  • Claims
  • Application Information

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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 polycaprolactone
  • A kind of preparation method of polycaprolactone
  • A kind of preparation method of polycaprolactone

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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 polycaprolactone, comprising the following steps: mixing a catalyst, an organic solvent and caprolactone, performing ring-opening polymerization reaction under the protection of anhydrous, oxygen-free and inert gas, and treating the reactant after the reaction To obtain polycaprolactone; 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 obtained polycaprolactone has a controllable molecular weight , 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 relates to an aminoanilinolithium compound and a preparation method thereof, and also relates to a method for preparing polycaprolactone by using the aminoanilinolithium compound as a catalyst. Background technique [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 people worry about 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, which has gradually increased the pollution of the human living environment. Traditional polymer materials are facing the tw...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/08C08G63/83C07C211/65C07C209/00
Inventor 徐征和王昕姚伟高爱红张云苹
Owner UNIV OF JINAN
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