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Carbon nitride-titanium nitride catalyst for synthesizing guaiacol, preparation method and application thereof

A titanium nitride catalyst, guaiacol technology, applied in physical/chemical process catalysts, chemical instruments and methods, dehydration of hydroxyl-containing compounds to prepare ether, etc., to delay carbon deposition, improve selectivity, and facilitate mass transfer. Effect

Active Publication Date: 2020-07-03
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Porous carbon nitride-titanium nitride composite materials have not been reported as catalysts in the system of gas-vicinol-methanol etherification to guaiacol

Method used

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  • Carbon nitride-titanium nitride catalyst for synthesizing guaiacol, preparation method and application thereof
  • Carbon nitride-titanium nitride catalyst for synthesizing guaiacol, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Zn modified porous carbon nitride-titanium nitride composite material, denoted as meso-ZnTiN / C, the preparation method is as follows:

[0039] (1) Prepare 600mL acetic acid aqueous solution (8wt%), add 60mL Ludox silicon oxide solution, 100g chitosan, 126g melamine, 340g n-butyl titanate and 30g zinc nitrate, fully stir at 30°C for 9h, and then add liquid at 100°C Evaporate to dryness to obtain block;

[0040] (2) The block was calcined at 800°C for 6h under a nitrogen atmosphere, the heating rate was 3°C / min, and then placed in an aqueous solution of ammonium bifluoride (5wt%) and stirred for 36h to remove the silica template, filtered, washed with distilled water, and dried at 120°C for 36h Then get meso-ZnTiN / C. The specific surface area of ​​the catalyst is 456m 2 / g, pore diameter ~ 20nm, ICP measurement of Ti, Zn content of 23.6%, 4.3%.

[0041] The meso-ZnTiN / C catalyst prepared above was used for gas-phase monoetherification of catechol and methanol to prepar...

Embodiment 2

[0043] The porous carbon nitride-titanium nitride composite material, denoted as meso-TiN / C, is prepared as follows:

[0044] (1) Prepare 400mL acetic acid aqueous solution (6wt%), add 40mL Ludox silica solution, 100g chitosan, 126g melamine and 272g n-butyl titanate, fully stir at 20°C for 12h, and evaporate to dryness at 80°C to obtain block shape;

[0045] (2) The block was calcined at 500°C for 8h under a nitrogen atmosphere, the heating rate was 1°C / min, and then placed in an aqueous solution of ammonium bifluoride (2wt%) and stirred for 60h to remove the silica template, filtered, washed with distilled water, and dried at 100°C for 60h Then get meso-TiN / C. The specific surface area of ​​the catalyst is 417m 2 / g, the pore diameter is ~16nm, and the Ti content is 26.8% as determined by ICP.

[0046] The meso-TiN / C catalyst prepared above was used for gas-phase monoetherification of catechol and methanol to prepare guaiacol. The specific steps are as follows: after loa...

Embodiment 3

[0048] Ce-modified porous carbon nitride-titanium nitride composite material, denoted as meso-CeTiN / C, is prepared as follows:

[0049] (1) Prepare 800mL acetic acid aqueous solution (10wt%), add 80mL Ludox silicon oxide solution, 100g chitosan, 126g melamine, 408g n-butyl titanate and 87g cerium nitrate, fully stir at 40°C for 6h, and add liquid at 120°C Evaporate to dryness to obtain block;

[0050] (2) The block was calcined at 1200°C for 4h under a nitrogen atmosphere, the heating rate was 6°C / min, and then placed in an aqueous solution of ammonium bifluoride (10wt%) and stirred for 12h to remove the silica template, filtered, washed with distilled water, and dried at 150°C for 12h Then get meso-CeTiN / C. The specific surface area of ​​the catalyst is 358m 2 / g, pore diameter ~ 12nm, ICP measurement Ti, Ce content is 28.2%, 6.5%.

[0051] The meso-CeTiN / C catalyst prepared above was used for gas-phase monoetherification of catechol and methanol to prepare guaiacol. The ...

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Abstract

The invention provides preparation of a hetero-element modified porous carbon nitride-titanium nitride (meso-MTiN / C) composite material, and a method for preparing guaiacol through gas-phase etherification of catechol-methyl alcohol by using the hetero-element modified porous carbon nitride-titanium nitride composite material. According to the catalyst, different nitrogen sources are used as raw materials, proper metal hetero-elements are selected for modification, the catalyst is synthesized through a chemical method, and the specific surface area can reach 300-500 m<2> / g; and the catalyst can catalyze catechol monoetherification to prepare guaiacol with high efficiency and high selectivity at a low temperature, wherein the conversion rate can reach 73% or above, the selectivity can reach97% or below, the service life can reach 3000 h, the stability is good, and the problem of catalyst carbon deposition inactivation in a gas phase fixed bed process is solved.

Description

technical field [0001] The invention belongs to the field of catalysts, and in particular relates to a carbon nitride-titanium nitride catalyst used for synthesizing guaiacol and its preparation method and use method. Background technique [0002] Guaiacol, also known as o-hydroxyanisole, o-i bhydroxyanisol, and methylcatechol, is an important fine chemical intermediate in industries such as spices, medicine, agriculture, and dyes . The biggest use of guaiacol is to produce vanillin, which is a precious broad-spectrum high-grade spice, which can be widely used as a deodorant, flavor-changing agent and flavoring agent in cosmetics, soaps, cakes, candies, beverages , tobacco and baked goods industries. As an important intermediate in organic synthesis, guaiacol can also be used to produce potassium guaiacol sulfonate, an expectorant and antitussive agent, and 5-nitroguaiacol sodium, a high-efficiency plant growth regulator. In addition, guaiacol can be used as an antioxidan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24C07C41/09C07C43/23
CPCB01J27/24C07C41/09C07C43/23
Inventor 林建东吴训锟李俊平王锐付松丁大康王勤隆黎源
Owner WANHUA CHEM GRP CO LTD
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