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Method for recovering methyl lactate by using supported ionic liquid as catalyst for alcoholysis of waste polylactic acid

A technology of ionic liquid and methyl lactate, which is applied in chemical instruments and methods, physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, etc., can solve the problem of large amount of ionic liquid, low purity, corrosion Equipment and other issues, to achieve good economic and environmental benefits, simple recycling process, to overcome the effect of corrosion equipment

Inactive Publication Date: 2019-06-28
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantages of the reported methods are that the traditional acid-base catalysts are difficult to recycle or reuse, corrode equipment, need to be neutralized and washed with water, resulting in a large amount of waste water and polluting the environment
Our research group reported that ionic liquid 1-alkyl-3-methylimidazole acetate (CN 2012101469065) and liquid Lewis acid (CN2015102531419) as catalysts can effectively catalyze the alcoholysis of PLA to recover corresponding products, but the separation of liquid catalysts is difficult , difficult to recycle
The amount of ionic liquid is large (the mass ratio of ionic liquid to PLA is generally 0.02-1:1, preferably 0.05-0.5:1;), although the amount of liquid Lewis acid is not large, they all contain transition metal salts, resulting in product color pollution, The purity is not high

Method used

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  • Method for recovering methyl lactate by using supported ionic liquid as catalyst for alcoholysis of waste polylactic acid
  • Method for recovering methyl lactate by using supported ionic liquid as catalyst for alcoholysis of waste polylactic acid
  • Method for recovering methyl lactate by using supported ionic liquid as catalyst for alcoholysis of waste polylactic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Catalyst preparation

[0032] (1) Preparation of [tespmim][Cl]

[0033] Put the refined 0.1mol N-methylimidazole in a 250mL three-necked round-bottomed flask, add 0.14mol 3-chloropropyltriethoxysilane (CPTES) dropwise under an ice-water bath, and stir the reaction at room temperature for 1.0h after the dropwise reaction, in N 2Under the atmosphere, heat, stir and reflux at 80°C for 72 hours, transfer the colorless viscous liquid to a 250mL separatory funnel while hot, wash the product with anhydrous ether (10mL×3) for several times to remove unreacted substances, pour the ether layer, the lower thick liquid was transferred to a 250mL single-necked flask, ether was removed by rotary evaporation, and vacuum-dried for 4.0h to obtain a light yellow viscous liquid [tespmim][Cl] with a yield of 91.4%.

[0034] (2) Preparation of [tespmim][OAc]

[0035] Put 0.07mol solid potassium acetate in a 100mL single-necked flask, add 30g of absolute ethanol, stir to dissolve to form ...

Embodiment 2

[0050] The experimental conditions and steps were the same as in Example 1, except that the reaction temperature was changed to 125° C., the conversion rate of PLA was 100%, and 5.55 g of methyl lactate was obtained with a yield of 96.0%.

Embodiment 3

[0052] Experimental condition and step are with embodiment 1, just with 0.04g catalyst [tespmim][OAc]-Zn(OAc) 2 / SBA was changed to 0.06g, the conversion rate of PLA was 100%, and 5.56g of methyl lactate was obtained, with a yield of 96.2%.

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Abstract

The invention discloses a method for recovering methyl lactate by using a supported ionic liquid [tespmim][OAc]-Zn(OAc)2 / SBA-15 as a catalyst for alcoholysis of a waste polylactic acid material (PLA).The method comprises the following steps that PLA, methanol and the catalyst [tespmim][OAc]-Zn(OAc)2 / SBA-15 are added into a reaction still for an alcoholysis reaction at 90-130 DEG C according to amass ratio of mPLA to mcatalyst and a molar ratio of nPLA to nmethanol, wherein the mass ratio of mPLA to mcatalyst is 1:(0.001-0.1), and the molar ratio of nPLA to nmethanol is 1:(1-10); after the reaction is completed, the catalyst is recovered by means of filtration, unreacted methanol is recovered by means of rotary distillation, and the product methyl lactate is collected by means of distillation under reduced pressure. The conversion rate of PLA can reach 100%, the yield of the product methyl lactate can reach 95% or above, the purity is 99%, and the catalyst supported ionic liquid [tespmim][OAc]-Zn(OAc)2 / SBA-15 can be directly reused.

Description

technical field [0001] The invention belongs to the technical field of high-value conversion of waste bio-based materials, and in particular relates to a method of catalyzing methanolysis of waste polylactic acid (PLA) with solid-supported ionic liquid catalyst [tespmim][OAc]-Zn(OAc)2 / SBA-15 Method for recovering methyl lactate. Background technique [0002] With the increase of population, the oil crisis and the continuous rise in the price of petrochemical-based raw materials, as well as the increasing attention of human beings to issues such as the environment and health, the development and utilization of renewable resources have attracted more and more attention. As a high-performance polymer material, polylactic acid (PLA) has the advantages of good biocompatibility, biodegradability, environmental friendliness and good mechanical properties. It is a petrochemical-based polymer such as polyester and polystyrene. It can be used as a potential substitute for biomaterial...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/03B01J31/02B01J35/10C07C69/68
Inventor 宋修艳王辉刘福胜卞兆荃于世涛刘仕伟
Owner QINGDAO UNIV OF SCI & TECH
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