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Preparation method of polycaprolactone

A technology for polycaprolactone and caprolactone is applied in the field of preparing polycaprolactone, which can solve the problems of difficulty in degrading polymer materials, aggravating pollution, and restricting the rapid development of polymer materials, and achieves controllable molecular weight and metal residues. Less, the effect of various catalyst structure changes

Inactive Publication Date: 2015-05-06
UNIV OF JINAN
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  • Summary
  • 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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  • Preparation method of polycaprolactone
  • Preparation method of polycaprolactone
  • Preparation method of polycaprolactone

Examples

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, add at -10°C, etc. The molar amount of n-butyllithium was slowly raised to room temperature to react for 3 hours, filtered and washed with dry n-hexane, collected and dried to weigh 0.49 g 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 H NMR (400 MHz, CDCl 3 ) δ 7.40 (d, J = 7.5 Hz, 2 H, Ph- H ), 7.24–6.91 (m, 10 H, Ph- H ), 6.62 (d, J = 7.6 Hz, 2 H, Ph- H ), 4.40 (s, 4H, C H 2 N), 2.72 (s, 12 H, NC H 3 ), 2.20 (s, 6 H, C H 3 ).

[0046] 13C NMR (100 MHz, CDCl 3 ) δ 152.45, 146.61, 134.27, 129.81, 128.23, 127.98, 126.66, 124.17, 116.34, 114.34, 48.86, 45.46, 20...

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 0.47 g of the ligand in 10 mL of dry cyclohexane, 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 0.46 g 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 H NMR (400 MHz, CDCl 3 ) δ 7.42 (dd, J = 6.2, 1.3 Hz, 2H, Ph- H ), 7.28-7.25 (m, 2H, Ph- H ), 7.17 (dd, J = 7.0, 1.0 Hz, 2H, Ph- H ), 7.06 (td, J = 7.4, 1.2 Hz, 2H), 7.00 (d, J = 7.4 Hz, 4H), 6.83 (t, J = 7.5 Hz, 2H), 4.17 (s, 4H, NC H 2 Ph), 2.73 (s, 12H, NC H 3 ), 2.31 (s, 12H, PhC H 3 ).

[0051]...

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 at -10°C Add 1.1 times the molar amount of methyllithium, rise to room temperature and react for 1 hour, filter and wash the filter cake with dry n-hexane, collect, dry and weigh to obtain 0.32 g, yield 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 H NMR (400 MHz, CDCl 3 ) δ 7.48–7.45 (m, 2H, Ph- H ), 7.29 (dd, J = 7.8, 1.5 Hz, 2H, Ph- H ), 7.19 (dd, J = 8.0, 1.1 Hz, 2H, Ph- H ), 7.13 (d, J = 7.9 Hz, 2H, Ph- H ), 7.09 (m, 4H, Ph- H ), 6.97 (dd, J = 8.1, 6.9 Hz, 2H, Ph- H ), 4.12 (s, 4H, NC H 2 Ph), 2.73 (s, 12H, NC H 3 ), 2.52 (q, J =...

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Abstract

The invention discloses a preparation method of polycaprolactone. The method comprises the following steps: mixing a catalyst, an organic solvent and caprolactone; carrying out ring-opening polymerization in the presence of anhydrous and anaerobic inert gases; treating a reactant to obtain polycaprolactone after reacting, wherein the catalyst is an amido anilino group lithium compound. With the amido anilino group lithium compound as a catalyst, the preparation method is good in reaction controllability, mild in condition, high in reaction rate and high in catalytic activity; polymerization reaction can be carried out without adding an alcohol-assisted catalyst; and the obtained polycaprolactone is controllable in molecular weight, high in productivity and few in metal residues. In addition, the polymerization reaction process is simple; a general solution polymerization method can be adopted; through control on polymerization reaction conditions, the molecular weight of the polymer can be regulated and controlled; and the obtained polymer is narrow in molecular weight distribution, has excellent physical and chemical characteristics, and can meet the requirements 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 Applications(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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