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Supercritical carbon dioxide dispersion polymerization stabilizer as well as preparation method and using method thereof

A technology of carbon dioxide and dispersion polymerization, applied in the production of bulk chemicals, etc., can solve the problem of difficult to meet requirements, high cost of stabilizers (such as fluorine-containing stabilizers and most siloxane-based stabilizers, toxic working pressure of stabilizers and other issues to achieve the effect of low cost

Inactive Publication Date: 2013-07-10
DALIAN UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these stabilizers are difficult to meet the requirements for industrial polymerization
The difficulties faced by these stabilizers in industrial production are: expensive stabilizers (such as fluorine-containing stabilizers and most silicone-based stabilizers), toxicity of the stabilizers themselves (such as fluorine-containing stabilizers) and work High pressure (most siloxane-based stabilizers and hydrocarbon stabilizers, the working pressure is usually 34.5MPa), etc.

Method used

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  • Supercritical carbon dioxide dispersion polymerization stabilizer as well as preparation method and using method thereof
  • Supercritical carbon dioxide dispersion polymerization stabilizer as well as preparation method and using method thereof
  • Supercritical carbon dioxide dispersion polymerization stabilizer as well as preparation method and using method thereof

Examples

Experimental program
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Effect test

example 1

[0034] Example 1. Add 3g of hydroxypropyl silicone oil and 3g of caprolactone to a pre-dried 100mL three-neck flask, add 80mL of anhydrous toluene, connect the water separator, and azeotropically remove water at 125°C under the protection of argon. When 50mL is evaporated Add 40 mg of stannous octoate after the toluene, continue to distill 4 mL of toluene, replace the water separator as a reflux device, and lower the temperature to 120 ° C for 24 hours. After the reaction, cool down to 20°C and add 6mL of dichloromethane to dissolve the product, slowly add dropwise to 10 times the volume of liquid methanol at -5°C to obtain a white solid product, add 6mL of dichloromethane to dissolve the product again, and use -5°C Liquid methanol was precipitated twice to remove unreacted monomers, and the product was dried in a vacuum oven at 30°C to constant weight to obtain the stabilizer PCL-b-PDMS-b-PCL, the product quality was 5.3g, and the yield It was 88.3%, and its final molecular w...

example 2

[0035] Example 2. Add 4.5g of hydroxypropyl silicone oil and 3g of caprolactone to a pre-dried 100mL three-necked flask, add 70mL of anhydrous toluene, connect the water separator, and azeotropically remove water at 130°C under the protection of argon. Add 50 mg of stannous octoate after 45 mL of toluene, continue to distill 3.5 mL of toluene, replace the water separator as a reflux device, and cool down to 120 ° C for 24 hours. After the reaction, cool down to 25°C and add 8mL of dichloromethane to dissolve the product, slowly add dropwise to 10 times the volume of 0°C liquid methanol to obtain a white solid product, re-add 8mL of dichloromethane to dissolve the product, and again use 0°C liquid methanol Precipitate twice to remove unreacted monomers, place the product in a vacuum oven at 30°C and dry to constant weight to obtain the stabilizer PCL-b-PDMS-b-PCL, the product quality is 6.5g, and the yield is 87.3 %, the final molecular weight determined by NMR calculation is 1...

example 3

[0036] Example 3. Add 2.5g of hydroxypropyl silicone oil and 2.5g of caprolactone to a pre-dried 100mL three-neck flask, add 75mL of anhydrous toluene, connect the water separator, and azeotropically remove water at 120°C under the protection of argon. After removing 50 mL of toluene, add 30 mg of stannous octoate, continue to distill 4 mL of toluene, replace the water separator as a reflux device, and lower the temperature to 100°C for 24 hours. After the reaction, cool down to normal temperature and add 5mL of dichloromethane to dissolve the product, slowly drop into 10 times the volume of -18°C liquid methanol to obtain a white solid product, add 5mL of dichloromethane to dissolve the product, and again use -18°C liquid Precipitate with methanol twice to remove unreacted monomers, place the product in a vacuum drying oven at 30°C and dry to constant weight to obtain the stabilizer PCL-b-PDMS-b-PCL, the product quality is 4.7g, and the yield is 93.3%, the final molecular wei...

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Abstract

The invention discloses a supercritical carbon dioxide dispersion polymerization stabilizer with a structure as polycaprolactone-b-polydimethylsiloxane-polycaprolactone. The stabilizer can be used for the synthesis of PLLA (Poly L Lactic Acid) at the reaction conditions of the reaction pressure of 19 MPA and the reaction temperature of 90 DEG C; the dosage of the stabilizer is 10%-3% of the weight of the polymerization reaction monomer; and the prepared product can be directly used for a drug sustained release system. The invention further discloses a method for preparing the stabilizer, wherein an ABA ternary segmented copolymer is prepared by using hydroxypropyl silicone oil and caprolactone as main materials through catalytic ring-opening of catalyst stannous octoate, wherein the weight ratio of the hydroxypropyl silicone oil to the caprolactone is (2:1) to (1:1). The stabilizer can be used for dispersion polymerization reaction of aliphatic polyesters including polyethyllactide, polycaprolactone and the like in a supercritical carbon dioxide. The preparation method is simple in process and environment-friendly, wherein the carbon dioxide can be recycled, so that the cost is low and the application prospect is good.

Description

technical field [0001] The present invention relates to dispersion polymerization in supercritical carbon dioxide, more specifically, to the synthesis of biomaterials polylactic acid (PLA), polyglycolide (PLGA), polycaprolactone (PCL), etc., and other functional materials Synthesis. Background technique [0002] Supercritical carbon dioxide (ScCO 2 ) has the characteristics of non-toxic, non-polluting, non-combustible, inert chemical reaction and low price. Moreover, it has good solubility to non-polar organic small molecules, has good swelling effect on polymers, can lower the glass transition temperature of polymers, and is beneficial to the progress of polymerization reaction. After the reaction is completed, the CO can be decompressed 2 Separated from the system, and during decompression, ScCO 2 The unique extraction function can extract unreacted monomers, initiators and stabilizers, avoiding the cumbersome post-processing procedures in traditional processes. There...

Claims

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Application Information

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IPC IPC(8): C08G63/06C08G63/08C08G63/78C08G77/445C08G63/695
CPCY02P20/54
Inventor 詹世平黄星赵启成
Owner DALIAN UNIVERSITY
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