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Bicyclic guanidine salt eutectic solvent catalyst as well as preparation method and application thereof

A low eutectic solvent, bicyclic guanidine technology, applied in the field of polymer plastic degradation, green/clean catalysis technology, can solve the problems of low reaction rate, harsh reaction conditions, difficulty in refining products, etc., to achieve stable catalyst, achieve yield, high yield effect

Active Publication Date: 2021-07-16
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Purpose of the invention: to design and develop a new type of green and efficient bicyclic guanidine salt deep eutectic solvent in view of the problems of low reaction rate, harsh reaction conditions and difficulty in refining products in the process of alcoholysis of waste PET in the prior art, which is not conducive to industrial implementation Catalysts to increase reaction rates and improve reaction conditions

Method used

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  • Bicyclic guanidine salt eutectic solvent catalyst as well as preparation method and application thereof
  • Bicyclic guanidine salt eutectic solvent catalyst as well as preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Add 20ml of deionized water into the Schleck reactor, and then add 2g of 1,5,7-triazidebicyclo(4.4.0)dec-5-ene. Heat and stir under the protection of high-purity nitrogen. After the system temperature reaches 30°C, add a 4% aqueous hydrochloric acid solution to the kettle dropwise from a constant pressure dropping funnel to control the 1,5,7-triazidebicyclo(4.4.0) The molar ratio of dec-5-ene to hydrochloric acid is 1:2 and stirred. The obtained product was rotary evaporated to remove the contained water, and the solid product was moved into a vacuum drying oven to dry for 48 hours to obtain 2.51 g of a white solid product, namely bicyclic guanidine chloride, with a yield of 98.4%. Then bicycloguanidine chloride and zinc acetate were mixed and stirred at a molar ratio of 1:1, the reaction temperature was 80° C., and the reaction time was 4 hours; the bicycloguanidine chloride / zinc acetate deep eutectic solvent was obtained.

Embodiment 2

[0030] Add 20ml of deionized water into the Schleck reactor, and then add 2g of 1,5,7-triazidebicyclo(4.4.0)dec-5-ene. Heat and stir under the protection of high-purity nitrogen. After the system temperature reaches 30°C, add 4% acetic acid aqueous solution to the kettle dropwise from a constant pressure dropping funnel to control 1,5,7-triazidebicyclo(4.4.0) The molar ratio of dec-5-ene to acetic acid is 1:1 and stirred. The obtained product was rotary evaporated to remove the contained moisture, and the solid product was moved into a vacuum drying oven to dry for 48 hours to obtain 2.49 g of a white solid product, ie, bicyclic guanidine acetate, with a yield of 96.2%. Then bicyclic guanidine acetate and zinc acetate were mixed and stirred at a molar ratio of 1:1, the reaction temperature was 80° C., and the reaction time was 4 hours; a bicyclic guanidine acetate / zinc acetate deep eutectic solvent was obtained.

Embodiment 3

[0032] Add 20ml of deionized water into the Schleck reactor, and then add 2g of 1,5,7-triazidebicyclo(4.4.0)dec-5-ene. Heat and stir under the protection of high-purity nitrogen. After the system temperature reaches 80°C, drop a 4% phosphoric acid aqueous solution into the kettle from a constant pressure dropping funnel to control the 1,5,7-triazidebicyclo(4.4.0) The molar ratio of dec-5-ene to phosphoric acid is 3:1 and stirred. The obtained product was rotary evaporated to remove the contained moisture, and the solid product was moved into a vacuum drying oven to dry for 48 hours to obtain 2.52 g of a white solid product, namely bicyclic guanidine phosphate, with a yield of 95.4%. Then bicyclic guanidine phosphate and zinc acetate were mixed and stirred at a molar ratio of 1:1, the reaction temperature was 80° C., and the reaction time was 4 hours; the bicyclic guanidine phosphate / zinc acetate deep eutectic solvent was obtained.

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Abstract

The invention discloses a bicyclic guanidine salt eutectic solvent catalyst as well as a preparation method and application thereof. The preparation method comprises the following steps of reacting 1, 5, 7-triazidobicyclo (4.4. 0) dec-5-ene with an acid solution to obtain bicyclic guanidine salt, and mixing with a hydrogen bond acceptor, and stirring for reaction to obtain the bicyclic guanidine salt eutectic solvent catalyst. By taking ethylene glycol as a solvent, degradation reaction is conducted on the bicyclic guanidine salt eutectic solvent catalyst and waste polyethylene glycol terephthalate to obtain the ethylene glycol terephthalate monomer. The catalyst has the advantages of simplicity in preparation, high catalytic activity, mild reaction conditions, short reaction time, high PET conversion rate, high BHET monomer selectivity, easiness in product separation, recyclability and green and pollution-free reaction process.

Description

technical field [0001] The invention belongs to the fields of green / clean catalysis technology and polymer plastic degradation, and in particular relates to a bicyclic guanidine salt deep eutectic solvent catalyst and its preparation method and application. Background technique [0002] Polyethylene terephthalate (PET) is a polyester material with excellent performance, which has comprehensive properties such as high strength, high rigidity, good heat resistance, and chemical resistance. Widely used in beverage bottles, fibers, films, substrates and electrical insulation materials and other fields. In 2020, the output of polyethylene terephthalate (PET) in my country will reach 53.5 million tons per year, and the waste PET resin produced every year will be as high as several million tons. With the rapid increase of PET production and sales, more and more waste PET will be generated. Although waste PET does not directly pollute the environment, it will occupy a large amount...

Claims

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Application Information

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IPC IPC(8): B01J31/04B01J31/02C07C67/03C07C69/82
CPCB01J31/04B01J31/0282C07C67/03B01J2231/49C07C69/82Y02W30/62
Inventor 江伟朱晨曦范楚梦孙平李爱民张全兴
Owner NANJING UNIV
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