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Method for preparing PCL-PDMS-PCL stabilizing agent by hydrogen chloride/ether solution catalysis

A PCL-PDMS-PCL, catalytic preparation technology, applied in the production of bulk chemicals, etc., can solve the problems of toxic side effects, long reaction time, etc., achieve mild reaction conditions, shorten reaction time, and avoid toxic and side effects

Inactive Publication Date: 2017-09-15
DALIAN UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, metal catalysts are mostly used in the preparation of dispersion stabilizers. The preparation method using metal catalysts takes a long time, generally takes 24-48 hours, and has toxic and side effects. Therefore, it is very important to develop stabilizers that are environmentally friendly, low in cost and have good anchoring effects.

Method used

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  • Method for preparing PCL-PDMS-PCL stabilizing agent by hydrogen chloride/ether solution catalysis
  • Method for preparing PCL-PDMS-PCL stabilizing agent by hydrogen chloride/ether solution catalysis
  • Method for preparing PCL-PDMS-PCL stabilizing agent by hydrogen chloride/ether solution catalysis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 5 g (0.0015 mol) of HTPDMS (0.0015 mol) that has been weighed, 30 mL of dichloromethane that has been dried and dehydrated, and 5 g (0.044 mol) of ε-CL into a 50 mL three-necked round-bottomed flask, and then add 4.2 mol / L of HCl·Et 2 O solution 0.71mL (0.003mol), stirred at 25°C for 4 hours, and protected by argon; after the reaction was completed, added to 300mL of cold methanol, filtered after the product was precipitated, and dried in vacuo to obtain the product PCL-PDMS-PCL8.6g, The molecular weight is 6384 g / mol, the yield is 86%.

Embodiment 2

[0022] Add 5 g (0.0015 mol) of HTPDMS (0.0015 mol) that has been weighed, 30 mL of dichloromethane that has been dried and dehydrated, and 5 g (0.044 mol) of ε-CL into a 50 mL three-necked round-bottomed flask, and then add 4.2 mol / L of HCl·Et 2 O solution 1.42mL (0.006mol), stirred at 25°C for 4 hours, and protected by argon; after the reaction was completed, added to 300mL of cold methanol, filtered after the product was precipitated, and dried in vacuo to obtain the product PCL-PDMS-PCL8.5g, The molecular weight is 6016 g / mol, the yield is 85%.

Embodiment 3

[0024] Add 5 g (0.0015 mol) of HTPDMS (0.0015 mol) that has been weighed, 30 mL of dichloromethane that has been dried and dehydrated, and 5 g (0.044 mol) of ε-CL into a 50 mL three-necked round-bottomed flask, and then add 4.2 mol / L of HCl·Et 2 O solution 0.71mL (0.003mol), stirred at 35°C for 4 hours, and protected by argon; after the reaction, added to 300mL of cold methanol, filtered after the product was precipitated, and dried in vacuo to obtain the product PCL-PDMS-PCL7.8g, The molecular weight is 6023 g / mol, the yield is 78%.

[0025] figure 2 It is the infrared spectrogram of the triblock stabilizer PCL-PDMS-PCL obtained in Example 1. at 3543cm -1 It is the stretching vibration peak of the terminal hydroxyl group (-OH) of the product, at 2961cm -1 and 2865cm -1 It is the C-H stretching vibration peak of the methylene group of PCL in PCL-PDMS-PCL, at 1735cm -1 It is the stretching vibration peak of the carbonyl group (C=O) in PCL, at 800cm -1 is the stretching v...

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Abstract

The invention relates to a method for preparing a PCL-PDMS-PCL stabilizing agent by hydrogen chloride / ether solution catalysis. The method comprises the following steps: initiating epsilon-caprolactone (epsilon-CL) ring opening polymerization by adopting hydroxypropyl terminated polydimethylsiloxane (HTPDMS) as an initiator and a hydrogen chloride / ether solution (HCL.Et20) as a catalyst to prepare a tri-block stabilizing agent polycaprolactone-b-polydimethylsiloxane-b-polycaprolactone (PCL-PDMS-PCL). Infrared spectroscopy and nuclear magnetic resonance hydrogen analysis indicate that the synthesized molecules are accordant with the structure of a target molecule. The optimized reacting conditions include a reacting temperature of 25 DEG C, a reacting time of 4 hours and a molar ratio of HCL.Et2O to HTPDMS being 2:1. The method can be used for solving a conventional problem caused by adopting a metal catalyst since the hydrogen chloride / ether solution is adopted as the catalyst, the preparation environment is environment-friendly, the reacting time is remarkably shortened, and the prepared tri-block stabilizing agent can be applied to a dispersing agent of biopharmaceutical polymerization in supercritical fluids.

Description

technical field [0001] The invention relates to the technical field of polymer polymerization, in particular to a method for preparing a PCL-PDMS-PCL stabilizer by catalyzing a hydrogen chloride / ether solution. Background technique [0002] Supercritical carbon dioxide (ScCO 2 ) technology has become a hot topic of research by many scholars. Because of its wide range of sources, gas-like diffusivity and liquid density, non-toxic, inert, and easy separation and purification of reaction products, it has become a green solvent instead of Many toxic and harmful organic solvents have been widely studied and applied, especially in the field of dispersion polymerization. [0003] Supercritical carbon dioxide can dissolve most low molecular weight non-polar molecules and some polar molecules, but most industrially widely used polymers cannot be dissolved under milder conditions, only amorphous fluoropolymers and Siloxane polymers are completely soluble in supercritical carbon diox...

Claims

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Application Information

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IPC IPC(8): C08G63/695C08G63/87
CPCC08G63/6952C08G63/823C08G63/87Y02P20/54
Inventor 詹世平邓进军王景昌侯维敏
Owner DALIAN UNIVERSITY
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