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Preparation method of polylactic acid functionalized graphene

A technology of polylactic acid and fossils, which is applied in the field of preparing polylactic acid functionalized graphene, can solve the problems of difficult interface bonding and low chemical activity, and achieve the effect of rich oxygen-containing functional groups, high grafting rate, and easy realization

Inactive Publication Date: 2013-05-08
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the large specific surface area and surface free energy of graphene, under the interaction of intermolecular forces, it is easy to form large aggregates, and graphene is a single carbon atom through sp 3 and sp 2 Hybrid composition, low chemical activity, it is difficult to form a firm and stable interfacial bond when compounded with polylactic acid matrix

Method used

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  • Preparation method of polylactic acid functionalized graphene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Firstly, graphite was prepared into graphite oxide according to the improved Hummers method. The specific method was to slowly add 21 g of flake graphite / potassium permanganate mixed solid with a mass ratio of 1:6 to 400 mL of H2O with a volume ratio of 9:1. 2 SO 4 / H 3 PO 4 In the mixed solution, after mixing evenly, place it in a constant temperature water bath at 50°C and continue to stir for 12 hours, then pour in H 2 o 2 Stand still in an ice bath for 24 hours, then repeatedly centrifuge and wash with deionized water until neutral, and then vacuum-dry at a temperature of 45° C. to obtain graphite oxide. The above-mentioned graphite oxide was prepared into a 1 mg / ml graphite oxide aqueous solution, then ultrasonically oscillated at room temperature for 2.5 hours to peel off the graphite oxide, and finally freeze-dried at a temperature of -50° C. to obtain powdered graphene oxide.

[0017] Then add 120ml of lactic acid into a 250ml reaction bottle, then place it ...

Embodiment 2

[0020] Graphene oxide was prepared by the method of Example 1.

[0021] Then add 120ml of lactic acid into a 250ml reaction bottle, then place it in an oil bath at 100°C, and conduct vacuum distillation and dehydration under a vacuum of 300Pa for 4 hours to obtain anhydrous lactic acid.

[0022] Then, 0.5 g of powdered graphene oxide and 0.3 g of stannous chloride as a catalyst were added to the above reaction flask, ultrasonically treated for 5 min, and then melted and polycondensed at a temperature of 170° C. and a vacuum of 70 Pa for 8 h. The reaction liquid was cooled, and then repeatedly dissolved with chloroform to wash away the polylactic acid not covalently bonded to graphene, and finally vacuum-dried at 50 °C for 24 h to obtain GO-g-PLA.

Embodiment 3

[0024] Graphene oxide was prepared by the method of Example 1.

[0025] Then add 120ml of lactic acid into a 250ml reaction bottle, then place it in an oil bath at 100°C, and conduct vacuum distillation and dehydration under a vacuum of 300Pa for 4 hours to obtain anhydrous lactic acid.

[0026] Then, 0.8 g of powdered graphene oxide and 0.3 g of stannous octoate as a catalyst were added to the above reaction flask, ultrasonically treated for 5 min, and then melted and polycondensed at a temperature of 170° C. and a vacuum of 70 Pa for 12 h. The reaction solution was cooled and dissolved repeatedly with chloroform to wash away polylactic acid not covalently bonded to graphene, and finally dried in vacuum at 50°C for 24 hours to obtain GO-g-PLA.

[0027] The present inventor has carried out the thermogravimetric analysis experiment to the GO-g-PLA that is prepared by the above-mentioned embodiment at the temperature of 30 ℃~700 ℃, under the protection of nitrogen, the thermogra...

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Abstract

The invention discloses a preparation method of polylactic acid functionalized graphene, which comprises the steps of preparing graphite oxide by adopting an improved Hummers method; performing ultrasonic peeling and freeze drying to obtain graphene oxide; mixing the graphene oxide with anhydrous lactic acid at certain proportion; adding a catalyst, and performing in-situ polymerization in vacuum environment to obtain a graphene / polylactic acid complex; and washing off the polylactic acid not in covalent binding with graphene to obtain polylactic acid functionalized graphene. The preparation method of polylactic acid functionalized graphene provided by the invention takes graphene oxide as an initiator and grafts polylactic acid to the surface of graphene oxide through lactic acid condensation polymerization by adopting a one-step method. The method does not need to perform pretreatment on graphene; the treatment process of lactic acid condensation polymerization is relatively simple and easy to realize, and the cost is relatively low. Moreover, the surface of graphene oxide is rich in oxygen-containing functional groups such as carboxyl group, hydroxyl group and the like; and relatively high grafting rate can be obtained through simple treatment.

Description

technical field [0001] The invention belongs to the technical field of modification of carbon nanomaterials, and in particular relates to a method for preparing polylactic acid functionalized graphene (GO-g-PLA) in one step by using graphene oxide (GO) as an initiator through polycondensation of lactic acid. Background technique [0002] Polylactic acid is a typical representative of biodegradable polymers. It belongs to poly-alpha hydroxy acid derivatives. It has good mechanical properties, biocompatibility and degradability, but its shortcomings such as poor toughness and low strength limit its wide application. application. Since its discovery in 2004, graphene has shown great potential in polymer reinforcement and toughening due to its excellent mechanical properties, ultra-high specific surface area and abundant functional groups on the surface. Studies have shown that adding a small amount of graphene can form a cross network structure in the polymer matrix, which can...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04C01B32/192C01B32/194
Inventor 徐志伟李文肖岳梦瑶单明景郭启微买巍杨彩云钱晓明
Owner TIANJIN POLYTECHNIC UNIV
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