Method for catalytic alcoholysis of PLA (Polylactic Acid) by CaO/MCF (Mesocellular silica Foam) mesoporous basic molecular sieve

A technology of molecular sieve catalyzing alcohol and polylactic acid, applied in molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of difficult separation of catalysts, complicated synthesis steps, harsh reaction conditions, etc., and achieves reusable performance. Good, simple recovery process, stable catalytic performance

Active Publication Date: 2017-11-24
QINGDAO UNIV OF SCI & TECH
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  • Abstract
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Problems solved by technology

[0005] In order to solve the shortcomings of catalysts existing in the prior art, such as difficulty in simple separation, poor reusability, cumbersome synthesis steps, high cost, large dosage, and harsh reaction conditions, the present invention provides a CaO / MCF mesoporous basic molecular sieve as Catalyst-catalyzed alcoholysis of waste polylactic acid by CaO / MCF mesoporous basic molecular sieve catalyzed alcoholysis of polylactic acid. This method is the first to apply a loaded solid base to the degradation of waste polylactic acid (PLA). The obtained product has high purity and at the same time The catalyst is stable in performance, environment-friendly, easy to separate, significantly avoids equipment corrosion, and can be reused well

Method used

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  • Method for catalytic alcoholysis of PLA (Polylactic Acid) by CaO/MCF (Mesocellular silica Foam) mesoporous basic molecular sieve
  • Method for catalytic alcoholysis of PLA (Polylactic Acid) by CaO/MCF (Mesocellular silica Foam) mesoporous basic molecular sieve
  • Method for catalytic alcoholysis of PLA (Polylactic Acid) by CaO/MCF (Mesocellular silica Foam) mesoporous basic molecular sieve

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Effect test

Embodiment 11

[0045] Catalyst preparation:

[0046] P 123 (EO20PO70EO20) (MW: 5000) was purchased from Sigma; orthoethyl silicate (TEOS), 1,3,5 trimethylbenzene (analytical pure) and tetrahydrate and calcium nitrate (analytical pure) were purchased from Shanghai Sinopharm Chemical Reagent Co., Ltd. Company; concentrated hydrochloric acid (HCl) (36%-38%) analytically pure, purchased from Laiyang Economic and Technological Development Zone Fine Chemical Plant.

[0047] Preparation of MCF: Weigh 2 g of commercially available P123 as a template, soak it in an aqueous HCl solution with a concentration of 1.6 mol / L, stir at 38°C for 2 hours until P 123 Dissolve completely, add 2g of mesitylene and 23mg of NH 4 F is a pore-enlarging agent. After continuing to stir for 2 hours, add 4.5g of TEOS (tetraethyl orthosilicate) dropwise and acidify for 24 hours, then transfer it to a hydrothermal synthesis kettle for crystallization at 100°C for 24 hours, and filter, wash and dry the product , roasting...

Embodiment 12

[0052] In an autoclave with a thermometer, add 5g of PLA in sequence (the molecular weight of PLA is 2.0×10 4 ~6.0×10 4 g / mol), 11.2g methanol, 0.83g CaO / MCF (prepared in Example 1.1), stirred and reacted (300 rpm) at 120°C for 3h, after the reaction, filtered under reduced pressure to filter out unreacted polylactic acid The unreacted methanol is recovered by atmospheric distillation at 70°C with the catalyst and filtrate, and the product methyl lactate is obtained by distillation under reduced pressure at 100°C. The product 6.2 g of methyl lactate was obtained. The alcoholysis rate of polylactic acid is 92%, and the selectivity of methyl lactate is 85.90%.

Embodiment 13

[0054] In an autoclave with a thermometer, add 5g of PLA, 11.2g of methanol, and 0.66g of CaO / MCF (prepared in Example 1.1) in sequence, and stir the reaction (300 rpm) at 125°C for 3h. Filtrate under reduced pressure to filter out unreacted polylactic acid and catalyst. The filtrate is distilled at 70°C under normal pressure to recover unreacted methanol, and then distilled under reduced pressure at 100°C to obtain the product methyl lactate. The product 6.1 g of methyl lactate was obtained. The alcoholysis rate of polylactic acid was 91.4%, and the selectivity of methyl lactate was 84.1%.

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Abstract

The invention discloses a method for the catalytic alcoholysis of (Polylactic Acid PLA) by a CaO/MCF (Mesocellular silica Foam) mesoporous basic molecular sieve, and belongs to the technical field of the high-value conversion of waste resources. The method is a reaction of degrading the PLA by using the CaO/MCF mesoporous basic molecular sieve as a catalyst and methanol as a reactant; after the reaction is finished, a methyl lactate product is recovered through operations of filtration, distillation and the like; the alcoholysis rate of the PLA can reach 98 percent or above; the selectivity of the product methyl lactate can reach 90 percent or above. According to the method, CaO/MCF is used as the catalyst; the methanol is used as a reactive raw material; a reaction condition is mild; a reaction method is simple; the price of the raw material is low; a process of recovering the product is simple; the catalyst can be repeatedly utilized; the degradation efficiency is high; the cost of degrading the PLA can be greatly industrially decreased; the method is actually an economical and effective way, and is worth popularizing.

Description

technical field [0001] The invention belongs to the technical field of high-value conversion of waste resources, and mainly relates to a method for catalyzing alcoholysis of waste polylactic acid by using CaO / MCF mesoporous basic molecular sieve as a catalyst. Background technique [0002] In recent years, with the rapid development of plastic, rubber and fiber industries that use petroleum as raw materials, the amount of energy storage on the earth is decreasing day by day, and the problem of environmental pollution is becoming more and more serious. All countries are considering sustainable development and environmental protection. How to solve these pollutions and develop new fiber materials that can be naturally degraded has become an important research goal of countries all over the world in recent years. Among them, degradable fiber materials processed from polylactic acid (PLA) have attracted special attention. Polylactic acid (PLA) is an excellent bio-based polymer ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/03C07C69/68B01J29/03
CPCB01J29/0308B01J2229/186C07C67/03C07C69/68
Inventor 刘福胜赵玉军宋修艳赵瑞阳
Owner QINGDAO UNIV OF SCI & TECH
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