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Synthetic method of fully-degradable multi-block copolymer and product thereof

A kind of technology of multi-block copolymer and synthesis method, applied in the field of synthesis of multi-block copolymer

Active Publication Date: 2014-06-18
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] So far, there have been no reports of directly catalyzing the "one-pot" reaction of multiple monomers to synthesize biodegradable carbon-oxo-bonded multi-block copolymers in large quantities.

Method used

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  • Synthetic method of fully-degradable multi-block copolymer and product thereof
  • Synthetic method of fully-degradable multi-block copolymer and product thereof
  • Synthetic method of fully-degradable multi-block copolymer and product thereof

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Experimental program
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Embodiment 1

[0059] The synthesis of embodiment 1 polyester-polycarbonate block copolymer

[0060] Before the reaction, the autoclave was dried in an oven at 110° C. for more than 3 hours, and then placed in a drying tower to cool down to room temperature naturally. Sequentially add 3.0mg Zn-Co III DMCC catalyst, 2.0ml CHO, 25.0mg stannous octoate (Sn(Oct) 2 ) catalyst, 50.0μl benzyl alcohol and 2.0ml CL, after sealing the reaction kettle, pressurize into 4.0Mpa CO 2 And quickly raise the temperature to 100°C, and after 5 hours of reaction, quickly cool down and release the pressure slowly. The crude product was subjected to CH 2 Cl 2 After washing with methanol and drying in vacuum, a yellow product was obtained, the conversion rate was calculated by weighing method, and the content of polycarbonate, polyester chain unit and polyether chain unit was calculated by hydrogen nuclear magnetic spectrum. The test results are shown in Table 1.

Embodiment 2

[0080] The synthesis of embodiment 2 polyester-polycarbonate block copolymers

[0081] Adopt the method of embodiment 1, difference is only in Zn-Co III The amount of DMCC catalyst used was 2.0 mg. The test results are shown in Table 1.

Embodiment 3

[0082]Synthesis of embodiment 3 polyester-polycarbonate block copolymer

[0083] Adopt the method of embodiment 1, difference is only in Zn-Co III The amount of DMCC catalyst used was 1.0 mg. The test results are shown in Table 1.

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Abstract

The invention discloses a synthetic method of a fully-degradable multi-block copolymer. The synthetic method of the fully-degradable multi-block copolymer comprises the following steps: adding a catalyst 1, a catalyst 2, an epoxide, a cyclic ester monomer and an initiator into a reactor, introducing CO2 into the reactor at a temperature of 40-120 DEG C till a pressure in the reactor is a pressure from a normal pressure to 5.0 MPa, then polymerizing and purifying to obtain the fully-degradable multi-block copolymer, wherein the catalyst 1 is zinc-cobalt double metal cyanide complex, zinc carboxylate, a diethylzinc-polyprotic system, a cobalt salicylaldimine or chromium complex, a zinc diimine complex or reduction large-cycle 2,6-salicylic aldehyde imine bizinc complex; the catalyst 2 is alkyl stannite, alkoxy zinc, alkoxy aluminum, salicylaldehyde imine alkyl aluminium, alkyl aluminium complex or organic alkali. By adopting a one-pot process, the multi-block copolymer with polyester blocks and polycarbonate blocks which are alternatively arranged is synthesized; the multi-block copolymer is excellent in thermal stability, biodegradability and mechanical property and adjustable in sizes and properties of soft and hard phases.

Description

technical field [0001] The invention belongs to the field of polymer material synthesis, and in particular relates to a method for synthesizing a fully degradable multi-block copolymer and a product thereof. Background technique [0002] Industrial "exhaust gas" carbon dioxide (CO 2 ) as a monomer, alternately copolymerized with epoxides under the action of a catalyst to synthesize biodegradable aliphatic polycarbonate (CO 2 base copolymer), which is a "green" route in line with the principles of low-carbon economy. reported CO 2 The main species of base polymers are linear polymers. such as CO 2 Polypropylene carbonate (PPC), an alternating copolymer of propylene oxide (PO), is a commercialized species with better biodegradability and comparable mechanical properties to polyethylene, but the glass transition temperature (T g ) is generally 35-40 ° C, hard and brittle at low temperature and soft at high temperature, it is difficult to use directly as an elastomer or pla...

Claims

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Application Information

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IPC IPC(8): C08G63/64
Inventor 张兴宏洪佳丽杜滨阳戚国荣
Owner ZHEJIANG UNIV