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A kind of preparation method of polyester containing carbon-carbon double bond

A technology of carbon double bond and polyester, which is applied in the field of preparation of carbon-carbon double bond polyester, can solve the problems of few modification points, low modification efficiency and difficult control, and achieve simple operation, controllable reaction and easy preparation Effect

Active Publication Date: 2020-05-01
HUANGSHAN SHENJIAN NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage is that the synthesis and purification methods of functional monomers are relatively complicated, and in most cases it also involves the protection and deprotection of functional side groups, which will cause the degradation of ester groups in the polyester main chain to a certain extent.
Post-polymerization modification is the functional modification of polyester polymers through chemical reactions. The disadvantages of this method are that there are few modification points to choose from, the modification efficiency is low and difficult to control, and there are also defects in the polyester main chain. The case of ester group degradation

Method used

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  • A kind of preparation method of polyester containing carbon-carbon double bond
  • A kind of preparation method of polyester containing carbon-carbon double bond
  • A kind of preparation method of polyester containing carbon-carbon double bond

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] Embodiment 1: synthesis contains the polycaprolactone of phenylselenyl group

[0055] Synthetic polycaprolactone containing phenylselenyl group, comprises the following steps:

[0056] Preparation of diphenyl diselenide (DPDS): install a thermometer, a constant pressure dropping funnel on a 250mL three-necked flask, and a spherical condenser with an anhydrous calcium chloride drying tube on the top. Weigh 2.4g (0.10mol) of magnesium chips and a catalytic amount of iodine into a three-necked flask, weigh 15.7g (0.10mol) of bromobenzene and 58mL of anhydrous ether into a constant pressure dropping funnel, and slowly drop them into the reactor. The reaction was exothermic, cooled in an ice-water bath to keep the reaction system slightly boiling, and continued to react at 35°C (boiling) for about 1 hour after the dropwise addition, and the magnesium chips basically reacted completely. Then 7.9g (0.10mol) of selenium powder was added in batches, and the reaction was refluxe...

Embodiment 2

[0061] Example 2: Research on PhSeCL Aggregation Behavior

[0062] In the glove box, add PhSeCL (0.5g, 1.8mmol), EG (6.2μL, 0.11mmol), Sn(Oct) in a 10mL ampoule 2 (36 μL, 0.11 mmol) and 2 mL of anhydrous toluene. Then the solution was divided into 5 parts in 2mL ampoules, and the tubes were sealed. The ampoules were then placed in a preheated 100°C heating plate and stirred for the set time. The solution was diluted with THF, precipitated in anhydrous ether, centrifuged to obtain the product, and dried in a vacuum oven at 25°C to constant weight. pass 1 H NMR was used to calculate the monomer conversion rate, and the molecular weight and molecular weight distribution of the polymer were measured by GPC.

[0063] attached Figure 4 The displayed GPC elution curve is unimodal and symmetrical. And attached Figure 5 The middle kinetics presents a pseudo first-order linear relationship, the molecular weight of the polymer increases linearly with the increase of the monomer ...

Embodiment 3

[0064] Example 3: Oxidation Reaction

[0065] According to the molar ratio of phenylselenyl group in the polymer: m-chloroperoxybenzoic acid=1:10, add the polymer, a certain amount of THF solvent, and m-chloroperoxybenzoic acid in a clean and dry 10mL ampoule, and stir at room temperature for 30 minutes Afterwards, ether was precipitated, centrifuged, and dried.

[0066] attached Figure 7 It can be seen from the GPC elution curve that the polymer peak shifts to a higher retention time. Due to the elimination of the phenyl selenide group, the molecular weight of the polymer changes from 9200g mol -1 Reduced to 7600g mol -1 , and the molecular weight distribution of the polymer is still very narrow It shows that the oxidation reaction has indeed occurred. attached Figure 8 After NMR oxidation, the resonance signal at chemical shift 7.60-7.15ppm disappeared, and the resonance signal at 3.63-3.46ppm on the methine group connected to selenium also disappeared, and at the sa...

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Abstract

The invention discloses a preparation method of a polyester containing carbon-carbon double bonds, and belongs to the technical field of polymer preparation. The preparation method uses a lactone containing a phenyl selenide group as a monomer to synthesize a polyester containing the phenyl selenide groups by homopolymerization or copolymerization, and then the polyester containing carbon-carbon double bonds in main chains is prepared by an oxidation reaction. The phenyl selenide group is introduced into the lactone structure by selecting and using suitable conditions in the preparation method, and functional double bonds are introduced into the polyester structure through the oxidation reaction, so that a diversified platform for polyester modifications is provided, and the application performance is preliminarily explored.

Description

technical field [0001] The invention relates to a preparation method of a carbon-carbon double bond-containing polyester, belonging to the technical field of polymer preparation. Background technique [0002] Polyester materials represented by polycaprolactone (PCL) have excellent biodegradability and biocompatibility, good flexibility and processability, and have great potential in the fields of tissue engineering materials, drug carrier materials and packaging materials. Wide application prospects. Functional materials based on polyester structure have long been one of the research focuses in industry and academia, and have developed rapidly in recent years. However, PCL polyester materials also have low strength, slow degradation, poor water solubility and no functional groups, which limit their application fields. Therefore, it is very necessary to modify it. [0003] Common polymer modification methods include physical modification and chemical modification. Compared...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/68C08G63/78
CPCC08G63/681C08G63/78
Inventor 朱健丁春来邢栋潘向强吴金安李娜朱秀林
Owner HUANGSHAN SHENJIAN NEW MATERIAL CO LTD
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