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Method for preparing aliphatic polyester

An aliphatic polyester and cyclic ester technology, which is applied in the field of polymer materials, can solve the problems of tin's poor health of children, weak polymer structure regulation ability, and high polymerization temperature, so as to improve quality, application safety, and polymer molecular weight. The effect of narrow distribution and low polymerization temperature

Inactive Publication Date: 2006-10-04
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Studies have shown that even the most widely used stannous octoate catalyst, which has been approved by the US FDA, the residual tin in the polymer may cause some cytotoxicity, and tin has extremely adverse effects on the health of young children
Although there are some non-toxic catalysts, their catalytic activity is often too low, the polymerization temperature is too high, and the ability to regulate the polymer structure is weak, so it is difficult to meet the practical requirements.
The contradiction between the catalytic activity and safety of ring-opening polymerization catalysts for cyclic ester monomers such as lactones and lactides has long restricted the development of high-quality biodegradable polymer materials and limited the further expansion of their application fields.

Method used

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  • Method for preparing aliphatic polyester
  • Method for preparing aliphatic polyester
  • Method for preparing aliphatic polyester

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preparation example Construction

[0018] In the preparation method of aliphatic polyester provided by the present invention, the cyclic ester monomer is selected from: glycolide, lactide, β-propiolactone, β-butyrolactone, γ-butyrolactone, γ -Any one of valerolactone, δ-valerolactone, ε-caprolactone, 1,4-dioxan-2-one, 1,5-dioxoheptan-2-one or a mixture thereof .

[0019] In the preparation method of the aliphatic polyester provided by the present invention, the cyclic ester monomer is preferably selected from glycolide, lactide, β-butyrolactone, δ-valerolactone, ε-caprolactone, 1 , any one of 4-dioxan-2-one, 1,5-dioxoheptan-2-one or a mixture thereof.

[0020] In the preparation method of aliphatic polyester provided by the present invention, the general structural formula of described metal-free N-heterocyclic carbene catalyst is:

[0021]

[0022] Among them, R 1 , R 3 selected from H atom, C 1 ~C 20 Alkyl, C 3 ~C 20 Branched chain alkyl, C 5 ~C 12 Cycloalkyl, Substituted Cycloalkyl, C 1 ~C 6 A...

Embodiment 1

[0046] Under anhydrous and oxygen-free conditions protected by high-purity nitrogen, mix 26 mg (0.1 mmol) of 1,3-dibutylimidazolium bromide (bbimBr) and potassium tert-butoxide 10 mg (0.09 mmol) uniformly, and fully React for 20 minutes to generate 1,3-di-n-butylimidazolcarbene (bbim) catalyst, then add monomer ε-caprolactone 1ml (9.4mmol) and initiator benzyl alcohol 10.8mg (0.1mmol), stir to make it mix uniform. After reacting at 25° C. for 30 minutes, a terminator water was added to terminate the reaction. 10 ml of tetrahydrofuran was added to dissolve the obtained polymer, and after precipitation, filtration and drying, polyε-caprolactone was obtained. The monomer conversion rate was 99.2%. The number average molecular weight measured by GPC is 9960, and the polydispersity index is 1.39. The molecular weight distribution curve of polyε-caprolactone is shown in figure 1 .

Embodiment 2

[0048] Under anhydrous and oxygen-free conditions protected by high-purity nitrogen, 10 mg (0.09 mmol) of potassium tert-butoxide was dissolved in 2 ml of tetrahydrofuran, and then 26 mg of substituted imidazolium salt 1,3-dibutylimidazolium bromide (bbimBr) was added ( 0.1 mmol), stirred to make it evenly mixed, reacted at 25° C. for 20 minutes, and filtered to obtain 1,3-di-n-butylimidazolecarbene (bbim) catalyst solution. Then, 1 ml (9.4 mmol) of monomer ε-caprolactone, 5 ml of tetrahydrofuran, and 10.8 mg (0.1 mmol) of benzyl alcohol were added, and stirred to make them evenly mixed. After reacting at 25° C. for 30 minutes, a terminator water was added to terminate the reaction. The obtained polymer solution is precipitated, filtered and dried to obtain polyε-caprolactone. The monomer conversion rate was 95.3%. The number average molecular weight measured by GPC is 8960, and the polydispersity index is 1.34.

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Abstract

The present invention discloses a preparation method of aliphatic polyester. It is characterized by that under the condition of inert atmosphere the cyclic ester monomer, metal-free N-heterocyctic carbene catalyst and alcoholic compound are uniformly mixed according to the mole ratio of 1:0.0002-0.2:0.0002-0.2 and reacted for 5 min to 24 hr at zero deg.C-150 deg.C so as to obtain the aliphatic polyester.

Description

technical field [0001] The present invention relates to polymer materials, in particular to a preparation method of aliphatic polyester Background technique [0002] Most polymer materials currently used, such as polyolefin, polystyrene, polyvinyl chloride, etc., are difficult to degrade naturally in nature, and their wastes have caused serious pollution to the environment, especially the so-called disposable plastics. "White pollution" urgently needs to find a solution. Aliphatic polyester is a kind of aliphatic polymer material with ester bonds on the main chain of its macromolecules. Under the action of water, enzymes or other microorganisms, the ester bonds on the main chain of the macromolecules are broken, and the molecular weight gradually decreases, forming It is a small molecular product, so it is a kind of polymer material that can be completely degraded. If biodegradable polymer materials are used instead of commonly used polymer materials such as polyolefins, t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/08
Inventor 吴林波李伯耿张海英
Owner ZHEJIANG UNIV
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