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Preparation method of bis-(5-formyl furfuryl)ether and polyamide material

A technology of formyl furfuryl and hydroxymethyl furfural, applied in the field of plastic processing, can solve the problems of limited large-scale application, poor hydrothermal stability, amorphization of pore walls, etc., and achieves good application prospects, small grain size, and pore size range. big effect

Pending Publication Date: 2020-06-05
ZHEJIANG SUGAR ENERGY TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Mesoporous molecular sieves in the prior art have problems such as poor hydrothermal stability, non-crystallization of pore walls, and weak acidity, which limit their large-scale application

Method used

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  • Preparation method of bis-(5-formyl furfuryl)ether and polyamide material
  • Preparation method of bis-(5-formyl furfuryl)ether and polyamide material
  • Preparation method of bis-(5-formyl furfuryl)ether and polyamide material

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0096] Embodiment 1 sample HZ-1 preparation

[0097] Add aluminum isopropoxide and tetrapropylammonium hydroxide to 60mL ethanol, stir at room temperature to form a clear solution A; add tetraethyl orthosilicate and hexadecyltrimethoxysilane to 30mL ethanol, Stir to form a clear solution B; add solution B dropwise to solution A, stir vigorously (1000 rpm) to form a uniform gel C, and the molar ratio of each material is 1SiO 2 :0.005Al 2 o 3 :0.2TPAOH:0.05HTS:30EtOH. The obtained gel C was dried in an oven at 25°C for 48 hours to obtain a dry gel, transferred to a hydrothermal kettle, added 70mL of deionized water, and crystallized in an oven at 170°C for 90 hours under steam-assisted conditions; Rinse the deionized product with deionized water, put the solid product in an oven, dry it at 100°C for 10 hours, then place it in a muffle furnace, and bake it at 550°C for 5 hours to obtain a hierarchical pore with a silicon-aluminum ratio of 100 Molecular sieve HZ-1.

Embodiment 2

[0098] Embodiment 2 sample HZ-2 preparation

[0099] Add aluminum isopropoxide and tetrapropylammonium hydroxide to 50mL ethanol, stir at room temperature to form a clear solution A; add tetraethyl orthosilicate and hexadecyltrimethoxysilane to 50mL ethanol, Stir to form a clear solution B; add solution B dropwise to solution A, stir vigorously (1000 rpm) to form a uniform gel C, and the molar ratio of each material is 1SiO 2 :0.01Al 2 o 3 :0.2TPAOH:0.05HTS:30EtOH. The obtained gel C was dried in an oven at 25°C for 48 hours to obtain a dry gel, transferred to a hydrothermal kettle, added 70mL of deionized water, and crystallized in an oven at 180°C for 80 hours under steam-assisted conditions; Rinse the deionized product with deionized water, put the solid product in an oven, dry at 100°C for 5 hours, then place it in a muffle furnace, and bake it at 550°C for 10 hours to obtain a hierarchical porous material with a silicon-aluminum ratio of 50 Molecular sieve HZ-2.

Embodiment 3

[0100] Embodiment 3 sample HZ-3 preparation

[0101] Add aluminum isopropoxide and tetrapropylammonium hydroxide to 60mL ethanol, stir at room temperature to form a clear solution A; add tetraethyl orthosilicate and hexadecyltrimethoxysilane to 40mL ethanol, Stir to form a clear solution B; add solution B dropwise to solution A, stir vigorously (1000 rpm) to form a uniform gel C, and the molar ratio of each material is 1SiO 2 :0.02Al 2 o 3 :0.2TPAOH:0.05HTS:30EtOH. The obtained gel C was dried in an oven at 30°C for 36 hours to obtain a dry gel, transferred to a hydrothermal kettle, added 60mL of deionized water, and crystallized in an oven at 190°C for 80 hours under steam-assisted conditions; Rinse the deionized product with deionized water, put the solid product in an oven, dry at 100°C for 5 hours, then place it in a muffle furnace, and bake it at 550°C for 7 hours to obtain a hierarchical porous material with a silicon-aluminum ratio of 25 Molecular sieve HZ-3.

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Abstract

The invention discloses a preparation method of bis-(5-formyl furfuryl)ether, which comprises the following steps: reacting a material containing 5-hydroxymethylfurfural in the presence of a catalystto prepare bis-(5-formyl furfuryl)ether; wherein the catalyst is a hierarchical pore ZSM-5 molecular sieve. The bis-(5-formyl furfuryl)ether is used as a raw material for preparing a polyamide material and has a wide application prospect.

Description

technical field [0001] The application relates to a preparation method of bis-(5-formyl furfuryl) ether and polyamide materials, belonging to the field of plastic processing. Background technique [0002] Bis-(5-formylfurfuryl)ether (OBMF) is an important bio-based chemical, on the one hand as an antiviral drug precursor, on the other hand for the preparation of imine-based polymers, especially as The raw materials are used to prepare polyamide materials; the latter can be widely used in aerospace materials, microelectronic devices, auto parts, coatings and other fields. Acid-catalyzed self-etherification of 5-hydroxymethylfurfural (HMF) is an effective method for the synthesis of OBMF. Compared with homogeneous acid catalysts, solid acid catalysts represented by molecular sieves can not only obtain higher OBMF yields, but also have the advantages of low corrosion, environmental protection, easy separation, and regeneration. In the prior art, mesoporous molecular sieves ha...

Claims

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Application Information

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IPC IPC(8): C07D307/46B01J29/40C08G12/12C08G69/40
CPCC07D307/46C08G69/40C08G12/12B01J29/40Y02P20/584B01J37/0018B01J37/036C01B39/40C01P2006/14C01P2006/12C01P2004/62B01J35/40B01J35/633B01J35/647B01J35/615
Inventor 王磊金海涛张建胡华雷杨勇卢国文
Owner ZHEJIANG SUGAR ENERGY TECH CO LTD
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