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Catalyst composition and preparation method of polylactide

A composition and catalyst technology, applied in the polymer field, can solve the problems of low molecular weight of polylactide, uncontrollable molecular weight, low polymer molecular weight, etc., and achieve the effect of high catalytic efficiency

Active Publication Date: 2021-01-19
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN1814645A discloses a preparation method and application method of a Schiff base aluminum catalyst for lactide ring-opening polymerization, but the catalytic activity of Schiff base aluminum is low, and the molecular weight of the polylactide finally obtained is low
The above catalysts all have high catalytic activity, but the molecular weight of the prepared polymer is low, and the molecular weight is uncontrollable

Method used

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  • Catalyst composition and preparation method of polylactide
  • Catalyst composition and preparation method of polylactide
  • Catalyst composition and preparation method of polylactide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] (1) Rare earth metal complex A (in formula (I), Ln is scandium, R is methyl, R 1 , R 2 , R 3 , R 4 are hydrogen, R 5 for the preparation of nitrate compounds)

[0053] The ligand structure is shown in formula (II), wherein R is a methyl group, R 1 , R 2 , R 3 , R 4 Both are hydrogen. Will be dissolved with 0.10mmol rare earth salt (Ln(R 5 ) 3 , Ln is scandium, R 5 Nitrate) in 2.0 mL of ethyl acetate solution was added dropwise to 2.0 mL of ethyl acetate solution in which 0.05 mmol of ligand was dissolved, a white precipitate was formed immediately, stirred at room temperature for 4 hours, centrifuged, washed with a small amount of ethyl acetate for 3 times, vacuum drying, yield 50%.

[0054] The elemental analysis data of the product is: C 62 h 50 N 10 o 12 Sc (found): C, 63.53 (63.52); H, 4.98 (4.98); N, 11.75 (11.77).

[0055] (2) Preparation of polylactide

[0056] At room temperature, add 10 μmol of rare earth metal complex A, 20 μmol of benzyl alc...

Embodiment 2

[0060] (1) The preparation of the rare earth metal complex is the same as in Example 1.

[0061] (2) Preparation of polylactide

[0062] At room temperature, add 10 μmol of rare earth metal complex A, 10 μmol of benzyl alcohol and 5 mL of toluene solvent into a 20 mL of anhydrous and oxygen-free polymerization bottle, react at 20°C for 5 minutes, add 40 mmol of lactide monomer, and stir at room temperature After 15 minutes, the ethanol solution of hydrochloric acid with a volume concentration of 10v% was added to terminate the reaction, the reaction solution was poured into ethanol for sedimentation, filtered to obtain a white solid, and the white solid was dried in a vacuum oven at 40°C for 48 hours to obtain a polylactide solid.

[0063] According to the nuclear magnetic resonance test, the conversion rate was 91%.

[0064] GPC analysis records the number average molecular weight M of polylactide n is 0.75 million, polydispersity coefficient M w / M n is 1.27.

Embodiment 3

[0066] (1) The preparation of the rare earth metal complex is the same as in Example 1.

[0067] (2) Preparation of polylactide

[0068] At room temperature, add 10μmol of rare earth metal complex A, 20μmol of benzyl alcohol and 50mL of toluene solvent into a 100mL anhydrous and oxygen-free polymerization bottle, react at 20°C for 5min, add 60mmol of lactide monomer, and stir at room temperature 1h, add ethanol solution of hydrochloric acid with a volume concentration of 10v% to terminate the reaction, pour the reaction solution into ethanol for sedimentation, filter to obtain a white solid, dry the white solid in a vacuum oven at 40°C for 48h to obtain a polylactide solid.

[0069] According to the nuclear magnetic resonance test, the conversion rate was 93%.

[0070] GPC analysis records the number average molecular weight M of polylactide n 188,000, polydispersity coefficient M w / M n is 1.19.

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Abstract

The invention relates to a catalyst composition, wherein the catalyst composition comprises a rare earth metal complex represented by a general formula (I) and a hydroxyl group-containing compound. The invention also relates to a preparation method of polylactide. The preparation method comprises the step of reacting a lactide monomer in an organic solvent containing the catalyst composition to obtain polylactide. The catalyst composition can efficiently catalyze polylactide synthesis, the molecular weight of polylactide can be controlled through the molar ratio of a rare earth metal complex to a hydroxyl-containing compound in the catalyst composition, and the molecular weight distribution is close to 1.

Description

technical field [0001] The invention belongs to the technical field of polymers, and in particular relates to a catalyst composition and a preparation method of polylactide. Background technique [0002] Polylactic acid (PLA) is a polyester biodegradable material with excellent biodegradability, so it is widely used in the production of tableware, film, fiber, clothing, auto parts and disposable containers, which is beneficial to solve the problem of petrochemical resource belt. to the problem of environmental pollution. In addition, polylactic acid also has the characteristics of good biocompatibility, non-toxicity and adjustable degradation. It meets the requirements of medical polymer materials. Controlled-release carrier materials and other aspects have broad application prospects. [0003] The early synthesis method of polyester was mainly based on the condensation reaction of acid compounds and alcohol compounds, but the structure of the polymer synthesized by this r...

Claims

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Application Information

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IPC IPC(8): C08G63/08C08G63/84C08G63/87
CPCC08G63/08C08G63/823Y02W90/10
Inventor 赵丽娜杜影齐可非唐伟刚
Owner CHINA PETROLEUM & CHEM CORP
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