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
View PDF0 Cites 16 Cited by
  • 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

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • 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
Comparison scheme
Effect test

Example Embodiment

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

Example Embodiment

[0035] Example 2. Add 4.5g of hydroxypropyl silicone oil and 3g of caprolactone into a pre-dried 100mL three-necked flask, add 70mL of anhydrous toluene, connect to a water separator, and azeotropically remove water at 130°C under the protection of argon. After 45 mL of toluene was added 50 mg of stannous octoate, 3.5 mL of toluene was continuously distilled out, the water trap was removed as a reflux device, and the temperature was lowered to 120°C for 24 hours. After the reaction, the temperature was lowered to 25°C and 8mL of dichloromethane dissolved product was added, and 10 times volume of 0°C liquid methanol was slowly added dropwise to obtain a white solid product. 8mL of dichloromethane dissolved product was added again, and 0°C liquid methanol was used again. Precipitate twice to remove unreacted monomers, and place the product in a vacuum drying oven at 30°C to dry to constant weight to obtain stabilizer PCL-b-PDMS-b-PCL. The product quality is 6.5g, and the yield is ...

Example Embodiment

[0036] Example 3. Add 2.5g of hydroxypropyl silicone oil and 2.5g of caprolactone into a pre-dried 100mL three-necked flask, add 75mL of anhydrous toluene, connect to a water separator, and azeotropically remove water at 120°C under the protection of argon. After 50 mL of toluene was added, 30 mg of stannous octoate was added, and 4 mL of toluene was continuously distilled out. The water separator was removed as a reflux device, and the temperature was lowered to 100°C for 24 hours. After the reaction, the temperature was lowered to room temperature and 5 mL of dichloromethane dissolved product was added, and 10 times volume of liquid methanol at -18℃ was slowly added dropwise to obtain a white solid product. 5 mL of dichloromethane dissolved product was added again, and the liquid at -18℃ was used again. Precipitate twice with methanol to remove unreacted monomers. Place the product in a vacuum drying oven at 30°C and dry to constant weight to obtain stabilizer PCL-b-PDMS-b-PCL...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
IPC IPC(8): C08G63/06C08G63/08C08G63/78C08G77/445C08G63/695
CPCY02P20/54
Inventor 詹世平黄星赵启成
Owner DALIAN UNIVERSITY
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap