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Preparation of metal-coated sulfonated nitrogen-doped carbon nanotube magnetic solid acid catalyst and application of metal-coated sulfonated nitrogen-doped carbon nanotube magnetic solid acid catalyst in synthesis of diphenolic acid

A magnetic solid acid and carbon nanotube technology, which is applied in the direction of catalyst activation/preparation, organic compound preparation, physical/chemical process catalysts, etc., can solve the problems of energy consumption, time-consuming, cumbersome process, etc., and achieve simple separation and preparation The effect of simple process and low cost

Active Publication Date: 2022-05-13
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The whole process is cumbersome, time-consuming and energy-consuming

Method used

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  • Preparation of metal-coated sulfonated nitrogen-doped carbon nanotube magnetic solid acid catalyst and application of metal-coated sulfonated nitrogen-doped carbon nanotube magnetic solid acid catalyst in synthesis of diphenolic acid
  • Preparation of metal-coated sulfonated nitrogen-doped carbon nanotube magnetic solid acid catalyst and application of metal-coated sulfonated nitrogen-doped carbon nanotube magnetic solid acid catalyst in synthesis of diphenolic acid
  • Preparation of metal-coated sulfonated nitrogen-doped carbon nanotube magnetic solid acid catalyst and application of metal-coated sulfonated nitrogen-doped carbon nanotube magnetic solid acid catalyst in synthesis of diphenolic acid

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Embodiment 1

[0037] The preparation method of the sulfonated nitrogen-doped carbon nanotube magnetic solid acid catalyst coated with metal cobalt in this embodiment comprises the following steps:

[0038] Step 1: Cobalt acetate, template agent and melamine were dissolved in water, and the resulting mixture was stirred at room temperature for 2 h, and further stirred at 80° C. for 0.5 h to obtain a suspension. Described cobalt acetate adopts [Co(CH 3 COO) 2 4H 2 O], the stencil agent is PEO-PPO-PEO, in which the mass ratio of cobalt acetate, stencil agent and melamine is 1:1.5:2.25; the mass ratio of cobalt acetate to water is 1:80.

[0039] Step 2: Remove the solvent in the suspension obtained in Step 1 by vacuum rotary evaporation, and calcinate the obtained powder at high temperature for 4-6 hours to obtain the calcined Co@NC. The calcined Co@NCs were further leached in an acid solution at 80 °C for 12 h, thoroughly washed with deionized water and dried to obtain Co@NCs. The calcinat...

Embodiment 2

[0042] The preparation method of the sulfonated nitrogen-doped carbon nanotube magnetic solid acid catalyst coated with metallic iron in this embodiment comprises the following steps:

[0043] Step 1: Ferric nitrate, template agent and melamine were dissolved in water, and the resulting mixture was stirred at room temperature for 2 h, and further stirred at 80° C. for 0.5 h to obtain a suspension. Described ferric acetate adopts [Fe(NO 3 ) 3 9H 2 O], the stencil agent is PEO-PPO-PEO, in which the mass ratio of ferric nitrate, stencil agent and melamine is 1:1.5:2.25; the mass ratio of ferric nitrate to water is 1:80.

[0044] Step 2: Remove the solvent in the suspension obtained in Step 1 by vacuum rotary evaporation, and calcinate the obtained powder at high temperature for 4-6 hours to obtain calcined Fe@NC. The calcined Fe@NC was further leached in an acid solution at 80°C for 12h, thoroughly washed with deionized water and dried to obtain Fe(@NC. The method of calcinati...

Embodiment 3

[0047] The preparation method of the sulfonated nitrogen-doped carbon nanotube magnetic solid acid catalyst coated with metal nickel in this embodiment comprises the following steps:

[0048] Step 1: Nickel nitrate, template agent and melamine were dissolved in water, and the resulting mixture was stirred at room temperature for 2 h, and further stirred at 80° C. for 0.5 h to obtain a suspension. Described nickel acetate adopts [Ni(NO 3 ) 2 ·6H 2 O], the stencil agent is PEO-PPO-PEO, wherein the mass ratio of nickel nitrate, stencil agent and melamine is 1:1.5:2.25; the mass ratio of nickel nitrate to water is 1:80.

[0049] Step 2: Remove the solvent in the suspension obtained in Step 1 by vacuum rotary evaporation, and calcinate the obtained powder at high temperature for 4-6 hours to obtain calcined Ni@NC. The calcined Ni@NC was further leached in an acid solution at 80 °C for 12 h, thoroughly washed with deionized water and dried to obtain Ni@NC. The calcination method...

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Abstract

The invention discloses preparation of a metal-coated sulfonated nitrogen-doped carbon nanotube magnetic solid acid catalyst and application of the metal-coated sulfonated nitrogen-doped carbon nanotube magnetic solid acid catalyst to synthesis of diphenolic acid, and the metal-coated sulfonated nitrogen-doped carbon nanotube magnetic solid acid catalyst is obtained by respectively encapsulating Fe, Co or Ni magnetic nanoparticles by nitrogen-doped carbon nanotubes modified by-SO3H groups. The magnetic nucleus of the magnetic catalyst is generated in situ in the roasting process, the synthesis step of traditional magnetic solid acid is greatly simplified, the packaging structure of the catalyst can effectively improve the stability of the catalyst and prolong the service life of the catalyst, and the magnetic catalyst can be applied to preparation of diphenolic acid by catalyzing condensation of levulinic acid and phenol and has a wide application prospect. The conversion rate of levulinic acid exceeds 99%, the yield of the obtained diphenolic acid exceeds 90%, and the isomer ratio (p, p ': o, p') of the diphenolic acid exceeds 20%.

Description

technical field [0001] The invention belongs to the technical field of bisphenol acid synthesis catalyst preparation, and in particular relates to the preparation of a metal-coated sulfonated nitrogen-doped carbon nanotube magnetic solid acid catalyst and its application in bisphenol acid synthesis. Background technique [0002] Bisphenol A (Bisphenol A, BPA) is used industrially to synthesize materials such as polycarbonate and epoxy resin. Since the 1960s, it has been used to make plastic (milk) bottles, suction cups for children, and coating the inside of food and beverage (milk powder) cans. BPA is everywhere, from mineral water bottles, medical equipment to the inside of food packaging. About 27 million tons of plastic containing BPA are produced worldwide each year. But BPA can also lead to endocrine disorders, which can lead to obesity, impaired male reproductive function, diabetes, cardiovascular and cerebrovascular diseases and even cancer. The European Union bel...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24B01J35/10C07C59/52C07C51/367
CPCB01J27/24B01J37/0018C07C51/367B01J35/33B01J35/398B01J35/40B01J35/61C07C59/52
Inventor 邓晋朱瑞彭远桃
Owner UNIV OF SCI & TECH OF CHINA
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