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Method for catalytic alcoholysis of poly-3-hydroxybutyrate by means of double-acid ionic liquid

A technology of hydroxybutyrate and ionic liquid, which is applied in the direction of chemical instruments and methods, catalytic reaction, reaction preparation of ester group and hydroxyl group, etc. It can solve the problems that the catalyst cannot be reused, the amount of waste water is large, and the equipment is corroded, so as to overcome the problem of catalyst The effects of corrosion equipment, stable catalyst performance, good economic and environmental benefits

Active Publication Date: 2017-09-22
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above traditional chemical depolymerization method needs to use a large amount of inorganic strong acid as a catalyst, the catalyst cannot be reused, the equipment is corroded, and it needs to be neutralized and washed, resulting in a large amount of wastewater

Method used

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  • Method for catalytic alcoholysis of poly-3-hydroxybutyrate by means of double-acid ionic liquid
  • Method for catalytic alcoholysis of poly-3-hydroxybutyrate by means of double-acid ionic liquid
  • Method for catalytic alcoholysis of poly-3-hydroxybutyrate by means of double-acid ionic liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] 1) Preparation of ionic liquid precursor

[0032] Add 36.6g of 1,3-propane sultone and 150mL of ethyl acetate into a three-necked flask, stir at a constant speed to form a clear and transparent solution, then slowly add 24.6g of N-methylimidazole dropwise into the three-necked flask, drop After the addition was completed, the mixture was stirred and heated to 50-55° C. for 2 hours, and the obtained white solid was washed with ethyl acetate several times, and vacuum-dried at 100° C. for 2 hours to obtain a white powdery solid.

[0033] 2) Preparation of functionalized ionic liquids

[0034] 20.4g ionic liquid precursor [HSO 3 -pmim] was placed in a three-necked flask, and distilled water was added to dissolve it into a transparent liquid, and then 0.11mol hydrochloric acid was slowly added dropwise at room temperature. After the dropwise addition was completed, the temperature was rapidly raised to 90°C, then stirred and refluxed for 2 hours, the water in the reaction ...

Embodiment 2

[0039] Step 1) and 2) are the same as in Example 1. Step 3) is:

[0040] 3) Preparation of ionic liquid

[0041] in N 2 Atmosphere, the [HSO 3 -pmim]Cl and FeCl 3 Add it into a three-neck flask at a molar ratio of 1:2, and heat and stir it. React for a period of time until it is completely melted to obtain the ionic liquid [HSO 3 -pmim]Cl-FeCl 3 (molar ratio 1:2).

Embodiment 3

[0043] Step 1) and 2) are the same as in Example 1. Step 3) is:

[0044] 3) Preparation of ionic liquid

[0045] in N 2 Atmosphere, the [HSO 3 -pmim]Cl and ZnCl 2 Add it into a three-necked flask at a molar ratio of 1:1, and heat and stir it. React for a period of time until it is completely melted to obtain the ionic liquid [HSO 3 -pmim]Cl-ZnCl 2 (molar ratio 1:1).

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Abstract

The invention provides a method for catalytic alcoholysis of poly-3-hydroxybutyrate by means of a Bronsted-Lewis double-acid ionic liquid. The method includes the steps that according to a molar ratio of nPHB to n catalysts as 1 to 0.01-0.1, poly-3-hydroxybutyrate and the catalyst Bronsted-Lewis double-acid ionic liquid are mixed, small molecular alcohol is added, and an alcoholysis reaction is conducted at 100-160 DEG C. According to the method for alcoholysis and recycling of poly-3-hydroxybutyrate with the Bronsted-Lewis double-acid ionic liquid as a catalyst to catalyze a waste material PHB, the product obtained with the method is high in purity, and the catalyst is stable in performance and can be repeatedly used. The conversion rate of the material PHB reaches 100%, the product yield reaches 92% or above, the recycled poly-3-hydroxybutyrate is an important chemical raw material, and excellent economic benefits and environmental benefits can be obtained by means of the method.

Description

technical field [0001] The invention belongs to the field of organic polymers, in particular to a method for catalyzing polyester degradation with an ionic liquid catalyst. Background technique [0002] Poly 3-hydroxybutyrate, also known as poly β-hydroxybutyrate (PHB for short), is polymerized from 3-hydroxybutyric acid monomer, can be thermoplastically formed, and can also be mixed with fiber, lignin, etc. to obtain a compound material and therefore versatile. With the rapid increase in production and sales of PHB materials, more and more waste PHB is produced. Although waste PHB materials can be degraded under natural conditions, the degradation cycle is too long and the degradation product CO 2 and H 2 O also causes a huge waste of resources because it cannot be recycled. Therefore, the research on recycling technology of waste PHB has been paid more and more attention by people. [0003] Currently, the reported chemical recycling methods are mainly divided into the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/03C07C69/675B01J31/30B01J31/26
CPCC07C67/03B01J31/0285B01J2231/49C07C69/675
Inventor 刘福胜宋修艳赵瑞阳于世涛刘仕伟王婵
Owner QINGDAO UNIV OF SCI & TECH
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