Preparation method of high-molecular-weight polylactic acid based on metal powder dehydrating agent

A high-molecular-weight, metal powder technology, applied in the field of preparation of high-molecular-weight polylactic acid, can solve problems that are difficult to eliminate, and achieve the effects of easy operation, simple conditions, and improved flame retardancy

Active Publication Date: 2013-08-21
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Aiming at the problem that small molecule water is difficult to eliminate in the later stage, the present invention relates to a kind of metal powder material that can react with water to remove the moisture in the system. Adding a small amount in the middle and late stage of lactic acid polycondensation can greatly promote the reaction process, and its product Does not affect polylactic acid used as a plastic

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 1) 300mL of 88% lactic acid aqueous solution was gradually heated up to 150°C under vacuum, and reacted for 24 hours to obtain a lactic acid prepolymer with a number average molecular weight of 262g / mol and a mass of 241.44g;

[0023] 2) Then add 1.2g of p-toluenesulfonic acid, 0.8g of stannous chloride and 0.4g of stannous octoate into the flask containing the lactic acid prepolymer, and connect the whole system to a reflux condenser, temperature control device and stirring On the device, gradually raise the temperature to 170°C under vacuum conditions, add a stirring blade after melting, add 0.4g of magnesium after 16-18 hours of reaction, and react for 6-8 hours to obtain the product polylactic acid with a weight average molecular weight of 15014g / mol.

Embodiment 2

[0025] 1) 300mL of 88% lactic acid aqueous solution was gradually heated to 150°C under vacuum, and reacted for 24 hours to obtain a lactic acid prepolymer with a number average molecular weight of 302g / mol and a mass of 210.30g;

[0026] 2) Then add 1.05g of p-toluenesulfonic acid, 0.7g of stannous chloride and 0.35g of stannous octoate into the flask containing 210.30g of lactic acid prepolymer, and connect the whole system to a reflux condenser and temperature control device On a stirring device, gradually raise the temperature to 170°C under vacuum conditions, add a stirring paddle after melting, and add 0.4g magnesium at the same time, and react for 24 hours to obtain the product polylactic acid with a weight average molecular weight of 12104g / mol.

Embodiment 3

[0028] 1) 300mL of 88% lactic acid aqueous solution was gradually heated to 150°C under vacuum, and reacted for 24 hours to obtain a lactic acid prepolymer with a number average molecular weight of 283g / mol and a mass of 220.68g;

[0029] 2) Then add 1.10g of p-toluenesulfonic acid, 0.73g of stannous chloride and 0.37g of stannous octoate into the flask containing 220.68g of lactic acid prepolymer, and connect the whole system to a reflux condenser and temperature control device On a stirring device, gradually raise the temperature to 170°C under vacuum conditions, add a stirring paddle after melting, and add 0.4g magnesium aluminum alloy powder at the same time, and react for 24 hours to obtain the product polylactic acid with a weight average molecular weight of 13607g / mol.

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Abstract

The invention relates to a preparation method of a high-molecular-weight polylactic acid based on a metal powder dehydrating agent, and belongs to the technical field of macromolecular materials. The method comprises the following steps of placing catalyst into the dehydrated prepolymer under a vacuum condition, controlling the reaction temperature at 160 to 180 DEG C, enabling the prepolymer and the catalyst to be reacted for 0 to 16 hours, and continuing the reaction for 1 to 24 hours after adding metal powder to obtain the product polylactic acid. The metal powder maerail which can be reacted with the water so as to remove the water in the system is adopted, the metal powder material is little added in the later stage of the polyconcentration of a lactic acid body, the water in the polyconcentration process can be efficiently removed, the reaction process can be greatly promoted, simplicity in operation can be realized, the repetition is good, the reaction efficiency is high, the preparation method is suitable for the dilated production, and the product is free from influencing the polylactic acid which is used as plastic.

Description

technical field [0001] The invention relates to a method for preparing high-molecular-weight polylactic acid based on a metal powder dehydrating agent, and belongs to the technical field of polymer materials. Background technique [0002] Polylactic acid is a new type of non-petroleum-based polymer material with good mechanical strength, chemical inertness and easy processing, and has good biodegradation and biocompatibility. Based on the non-toxic and non-irritating biocompatibility of polylactic acid to the human body, the US Food and Drug Administration (FDA) has approved materials for use in the medical field. It is currently widely used in medical implants, surgical sutures, drug controlled release systems, and fractures. Internal fixation, tissue regeneration and other fields. It can replace petroleum-based plastics in a certain range. At the same time, polylactic acid has very similar physical and mechanical properties to general-purpose plastics, and can replace no...

Claims

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Application Information

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IPC IPC(8): C08G63/06C08G63/78C08K3/08C08L67/04C08K3/22
Inventor 杨荣杰尹梦岩邹美帅郭晓燕
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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