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Poly D-lactic acid-isopropylidene glucose diblock copolymer material and preparation method thereof

A technology of diblock copolymer and isopropylidene group is applied in the field of poly-D-lactic acid-isopropylidene glucose diblock copolymer material and its preparation, which can solve the problem of unstable performance, difficult to control copolymer performance, The number of PLA segments is difficult to control, etc.

Inactive Publication Date: 2020-04-17
NANJING FORESTRY UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] When monosaccharides and polysaccharides are copolymerized to modify polylactic acid, because the sugar molecules contain more hydroxyl groups, it is difficult to control the molecular chain structure of the copolymer, and the properties of the obtained copolymer are also difficult to control, resulting in unstable performance of the material
Among them, glucose contains 5 hydroxyl groups. When copolymerized with PLA, all hydroxyl groups may participate in the reaction. Therefore, it is difficult to control the number of hydroxyl groups of glucose in the copolymer and the number of PLA chain segments, resulting in unstable performance.

Method used

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  • Poly D-lactic acid-isopropylidene glucose diblock copolymer material and preparation method thereof
  • Poly D-lactic acid-isopropylidene glucose diblock copolymer material and preparation method thereof
  • Poly D-lactic acid-isopropylidene glucose diblock copolymer material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] use as figure 2 The synthetic route shown prepares poly-D-lactic acid-isopropylidene glucose diblock copolymer. (1) Preparation of 1,2;5,6-oxo-diisopropylidene glucose (IPG) by hydroxyl protection method. Add 10 g of glucose and 200 ml of acetone into the reactor, stir and add an appropriate amount of zinc chloride and phosphoric acid (the molar ratio of which is 1:0.1) in sequence, and react for 30 h at room temperature and normal pressure. Add 50% NaOH aqueous solution dropwise under rapid stirring to adjust the pH of the reaction system to 8.0, filter with suction, wash with acetone for 2 to 3 times until the filtrate is colorless and transparent, rotary evaporate the filtrate, dissolve the obtained solid in chloroform, wash and extract with water 2 to 3 times, the obtained chloroform solution was rotary evaporated, and the obtained sample was recrystallized 2 to 3 times with ethyl acetate and petroleum ether to obtain white needle-shaped IPG. (2) Preparation of p...

Embodiment 2

[0023]The method in Example 1 was used to prepare IPG. Weigh 100g of D-lactic acid and add it to the reactor, heat up to 150°C, react at normal pressure and constant temperature for 1h, then depressurize to 200Pa and react for 4h, then add the catalyst stannous isooctanoate (0.5wt% of PDLA), and heat up to React at 180°C for 10h under reduced pressure to below 10Pa to obtain poly-D-lactic acid, then add IPG to the reaction system, the molar ratio of IPG to PDLA is 8:1, and react at 10Pa and 200°C for 6h. The obtained product was dissolved in chloroform, excess methanol was precipitated, and the precipitate was vacuum-dried to obtain poly-D-lactic acid-isopropylidene glucose diblock copolymer. use 1 H-NMR spectrum (such as image 3 Shown) analysis of the resulting copolymer molecular chain has PDLA and IPG diblock structure (such as figure 1 shown). The weight-average relative molecular mass of the diblock copolymer is 36000, and the specific rotation [α] 25 D It is about...

Embodiment 3

[0025] The method in Example 1 was used to prepare IPG. The D-lactic acid that takes by weighing 100g is added in the reactor, is heated up to 150 ℃, normal pressure constant temperature reaction 1h, then depressurizes to 200Pa reaction 4h, then adds catalyst tin protochloride (mass is 0.3wt% of PDLA), heats up to React at 180°C for 6 hours under reduced pressure below 10Pa to obtain poly-D-lactic acid, then add IPG to the reaction system, the molar ratio of IPG to PDLA is 10:1, and react for 8 hours at 10Pa and 200°C. The obtained product was dissolved in chloroform, excess methanol was precipitated, and the precipitate was vacuum-dried to obtain poly-D-lactic acid-isopropylidene glucose diblock copolymer. use 1 The diblock copolymer molecular chain obtained by H-NMR spectrum analysis has PDLA and IPG diblock structure (molecular chain structure such as figure 1 shown). The weight-average relative molecular mass of the diblock copolymer is 28000, and the specific rotation ...

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Abstract

The invention discloses a poly D-lactic acid-isopropylidene glucose diblock copolymer material and a preparation method thereof, and belongs to the technical field of high polymer materials. The diblock copolymer material is prepared by taking poly D-lactic acid and hydroxyl-protected diisopropylidene glucose as raw materials, carrying out a melt polymerization reaction for 4-12 h under the conditions that the pressure is 10-300 Pa and the temperature is 160-200 DEG C when the molar ratio of 1,2;5,6-oxo-diisopropylidene glucose to the poly D-lactic acid is larger than 4:1. The diblock copolymer material has a specific rotation [alpha] 25D of about +145, a melting temperature of about 148 DEG C, and a crystallinity of about 49%, which are similar to those of poly D-lactic acid, but the copolymer material has a hydrophilicity superior to that of poly D-lactic acid, a contact angle of about 72 degrees, and a contact angle of 85 degrees.

Description

Technical field: [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a poly-D-lactic acid-isopropylidene glucose diblock copolymer material and a preparation method thereof. Background technique: [0002] Polylactic acid (PLA) is a bio-based green thermoplastic derived from biomass that can eventually decompose into carbon dioxide, water and humus. PLA includes two optical isomers of poly-L-lactic acid (PLLA) and poly-D-lactic acid (PDLA). The specific rotation of PLLA is -160, while the specific rotation of PDLA is +160, and its optical activity has a great influence on the performance of PLA. have a significant impact. PLA has good degradability and mechanical properties, and can be used in biomedicine, packaging, textile fibers and other fields. However, polylactic acid has poor heat resistance and low hydrophilicity, which limit its application. Therefore, PLA needs to be modified to improve its performance. Copolyme...

Claims

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Application Information

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IPC IPC(8): C08G63/91C08G63/08C07H1/00C07H9/04
CPCC07H1/00C07H9/04C08G63/08C08G63/912
Inventor 高勤卫朱前进祁俐燕刘婷婷常开新曹丹
Owner NANJING FORESTRY UNIV
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