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Method for end capping carbon dioxide-epoxide copolymer with polymer end-capping reagent containing anhydride structural unit

A technology of carbon dioxide and epoxy, which is applied in the field of capping carbon dioxide-epoxide copolymers with polymer capping agents containing acid anhydride structural units, which can solve problems such as difficult control of capping temperature and dosage, volatile environment, pollution, etc. , to achieve the effect of being beneficial to industrial processing and utilization, widening the processing window, and overcoming environmental pollution

Active Publication Date: 2012-01-25
CHANGZHOU INST OF ENERGY STORAGE MATERIALS &DEVICES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, the end-capping agents given in patents and literatures all belong to the category of "small molecules", and these "small molecule end-capping agents" are difficult to adapt to the melting end-capping during the processing of carbon dioxide-epoxide copolymers, not only It is difficult to control the capping temperature and dosage during the melting reaction process, and these "small molecule" capping agents cause environmental pollution due to their volatility during the melt blending capping process, and unreacted "small molecules" during the cooling process The capping agent is easy to precipitate on the surface of the melt

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation Embodiment 1

[0027] Preparation Example 1: Under the protection of nitrogen, add 1.84 g of sublimed maleic anhydride to a 250 ml three-necked flask that was evacuated three times to 20-40 Pa and filled with nitrogen, and inject 15.4 g of maleic anhydride treated with CaH 2 Reflux treated anhydrous toluene, when the temperature in the bottle was heated to 85°C and kept constant for 20 minutes, under stirring at 250rpm, add 16.92% benzoyl peroxide containing 0.094g benzoyl peroxide dropwise through the constant pressure dropping funnel g methyl methacrylate solution, the reaction temperature is controlled at 85±2°C during the dropwise addition, and the dropwise addition is completed within 40 minutes. After the dropwise addition was completed, the reaction was continued at 85° C. for 8 hours. After the polymerization reaction, 0.13 g of antioxidant 1010 was added to the reactant and stirred for 20 minutes, and then the reactant was distilled under reduced pressure at 110° C. and 1.33 KPa unt...

preparation Embodiment 2

[0028] Preparation Example 2: Under nitrogen protection, 1.09 g of sublimated maleic anhydride was added to a 250 ml three-necked flask that was evacuated three times to 20-40 Pa and filled with nitrogen, and 23.22 g of it was injected with CaH 2 Reflux treated anhydrous toluene. When the temperature in the bottle was heated to 90° C. and kept constant for 20 minutes, under stirring at 250 rpm, 13.28 g of isooctyl methacrylate containing 0.144 g of lauroyl peroxide and The mixed solution of 14.48g methyl methacrylate, during the dropwise addition, the reaction temperature is controlled at 90±2°C, and the dropwise addition is completed within 60 minutes. After the dropwise addition was completed, the reaction was continued at 90° C. for 9 hours. After the polymerization reaction, 0.15 g of antioxidant 1010 was added to the reactant and stirred for 20 minutes, and then the reactant was distilled under reduced pressure at 110° C. and 1.33 KPa until no residual liquid dripped out...

preparation Embodiment 3

[0029] Preparation Example 3: Preparation of rare earth three-way catalyst for carbon dioxide-epoxide copolymerization.

[0030] at 99.99% CO 2 Under the protection of 80 ℃, evacuate to 20 ~ 40Pa and fill with CO 2 A total of 6 times of CO charging after 2 hours of treatment 2 In the rare earth three-way catalyst configuration bottle, add 0.00097mol Y(CCl 3 COO) 3 , 40ml 1,3-dioxolane and 0.0097mol glycerol, to be Y (CCl 3 COO) 3 After all dissolved, add 0.01954molZnEt dropwise to the configuration bottle 2 , ZnEt 2 The rate of addition of the solution is controlled between 35 and 45°C with the reaction temperature in the bottle. ZnEt 2 After the dropwise addition, fully shake the catalyst configuration bottle by hand until no more gas is released. The catalyst preparation bottle was placed in a constant temperature bath for aging treatment. The aging conditions were: 60° C.; the mechanical oscillation frequency was 150 times / min, the amplitude was 40 mm, and the mech...

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PUM

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Abstract

The invention relates to a method for end capping carbon dioxide-epoxide copolymer with polymer end-capping reagent containing anhydride structural units, which not only can effectively overcome the defects that estolide and other small molecule end-capping reagent are easy to be volatilized when end-capping carbon dioxide-epoxide copolymer through melt blending reaction, the environment is polluted, and the small molecule end-capping reagent is easy to be separated out on the surface when the fusant is cooled, and the like; and in addition, compared with end capping carbon dioxide-epoxide copolymer with the small molecule end-capping reagent, end capping carbon dioxide-epoxide copolymer with polymer end-capping reagent containing anhydride structural units can obtain better thermal stability, and the thermal decomposition temperature is improved by 20 to 35DEG C.

Description

technical field [0001] The invention belongs to a method for capping a carbon dioxide-epoxide copolymer with a high molecular capping agent containing an acid anhydride unit. Background technique [0002] Carbon dioxide-epoxide copolymers have attracted much attention due to their excellent barrier properties, good biocompatibility, biodegradability, and good physical and mechanical properties. Due to the poor thermal stability of carbon dioxide-epoxide copolymers, it is easy to "unzip" thermal degradation reactions from the end of the molecular chain during processing, making its physical and mechanical properties worse. Therefore, people have been exploring carbon dioxide for many years. - End-capping method for epoxy copolymers, seeking to improve thermal stability of carbon dioxide-epoxide copolymers. [0003] Dixon once proposed to cap the carbon dioxide-epoxide copolymer in solution form with an organic compound that is easy to react with hydroxyl (US4066630; US410426...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G81/02C08G64/34C08F220/14C08F220/18C08F222/06B29B7/00B29C47/92B29C48/40B29C48/92
CPCB29C48/92B29C2948/92704B29C48/40B29C48/625B29C48/9185B29C2948/9259B29C2948/92885B29C2948/92895B29C2948/92904
Inventor 赵晓江王献红王佛松周庆海董艳磊闵加栋乔立军高凤翔
Owner CHANGZHOU INST OF ENERGY STORAGE MATERIALS &DEVICES
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