Method for preparing poly-oxalate-1,4-butylene

A technology of butanediol ester and diethyl oxalate, applied in the field of polyoxalic acid-1, can solve problems such as high cost and long reaction time, and achieve the effects of low cost, simple operation and reduction of reaction vacuum degree

Inactive Publication Date: 2011-10-19
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] For the high cost of poly-1,4-butylene oxalate and the long defect of reaction time in the prior art, the object of the present invention is to provide a kind of preparation method of poly-1,4-butylene oxalate, described Poly-1,4-butanediol oxalate is prepared by copolymerization of diethyl oxalate and 1,4-butanediol, which are derived from biomass, have low cost and high thermal stability

Method used

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  • Method for preparing poly-oxalate-1,4-butylene

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Embodiment 1

[0036] Weigh respectively 0.5mol of diethyl oxalate (73.07g), 0.5mol of 1,4-butanediol (45.06g) and 0.005mol of sodium methoxide, add in a 500ml three-necked round-bottomed flask, pass into N 2 , the flow rate is 0.1m 3 / h, heated in an oil bath to control the reaction temperature at 140°C, stirred mechanically, and the reactants were completely melted. When the reaction temperature rose to 140°C, the timing was started, and the reaction was carried out at a constant temperature for 5 hours. The obtained product was a dark white solid with an intrinsic viscosity of 0.04dL / g.

[0037] figure 1 The crystallization curve in the DSC spectrogram of the poly-1,4-butanediol oxalate prepared for the present embodiment is obtained by figure 1 It can be seen that the crystallization temperature of the product of this example is 55.9°C.

[0038] figure 2 The melting curve in the DSC spectrogram of the poly-1,4-butanediol oxalate prepared for the present embodiment is obtained by fi...

Embodiment 2

[0043] Weigh 0.5mol of diethyl oxalate, 0.5mol of 1,4-butanediol and 0.005mol of NaOH respectively, add them to a 500ml three-necked round-bottomed flask, and inject N 2 , the flow rate is 0.1m 3 / h, heating in an oil bath to control the reaction temperature at 140°C, stirring mechanically, the reactants are completely melted, when the reaction temperature rises to 140°C, start timing, and react at a constant temperature for 5h, and the product obtained is poly-1,4-butylene oxalate. It is a dark white solid with an intrinsic viscosity of 0.04dL / g.

Embodiment 3

[0045] Weigh respectively 0.5mol of diethyl oxalate, 0.5mol of 1,4-butanediol and 0.005mol of KOH, add to a 500ml three-necked round-bottomed flask, and inject N 2 , the flow rate is 0.1m 3 / h, heating in an oil bath to control the reaction temperature at 140°C, stirring mechanically, the reactants are completely melted, when the reaction temperature rises to 140°C, start timing, and react at a constant temperature for 5h, and the product obtained is poly-1,4-butylene oxalate. It is a dark white solid with an intrinsic viscosity of 0.06dL / g.

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Abstract

The invention relates to a method for preparing poly-oxalate-1,4-butylene, and belongs to the technical field of high polymer materials. The method comprises the following steps of: putting diethyl oxalate, 1,4-butanediol and a catalyst into a reactor, and reacting at the constant temperature of between 80 and 170 DEG C with stirring under the protection of N2 with the flow of between 0.06 and 0.16 m<3>/hour for 0.5 to 5 hours to obtain the poly-oxalate-1,4-butylene, wherein a ratio of the diethyl oxalate to the 1,4-butanediol is 1:1-1:3; and the catalyst is oxalic acid preferably, and the catalyst is 0.1 to 5.0 molar percent based on the diethyl oxalate. In the method, the diethyl oxalate and the 1,4-butanediol also can react at the constant temperature of between 110 and 180 DEG C under the vacuum degree of between 200 and 500 Pa under constant pressure for 3 to 8 hours in the presence of the catalyst to obtain the poly-oxalate-1,4-butylene with higher intrinsic viscosity. By the method, the reaction time is shortened, the vacuum degree of the reaction is reduced, the cost is low, and operation and aftertreatment are simple, so the method is suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation method of poly-1,4-butylene oxalate (Poly(Butylene Oxalate), PBO), which belongs to the technical field of polymer materials. Background technique [0002] Traditional plastics are derived from non-renewable petroleum resources and are difficult to degrade, causing white pollution. Therefore, the development of non-petroleum-based biodegradable plastics to replace traditional plastics is of great significance to the sustainable development of the plastics industry and the protection of the ecological environment. [0003] Aliphatic polyester has good biodegradability and is a research hotspot of biodegradable plastics. The main problems of biodegradable aliphatic polyesters are mechanical properties and cost. More researched aliphatic polyesters include polylactic acid (PLA), polyhydroxyalkanoate (PHA), poly(ε-caprolactone) (PCL), polypropylene carbonate (PPC), polybutylene succinate Glycol ester (PBS) and poly...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/16C08G63/78
Inventor 张青山宁卓远李云政武钦佩尹宏权马东霞
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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