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Preparation method of ceramic surface supported catalytic filler

A technology of catalytic packing and ceramic surface, which is applied in the cross-application field of materials and chemical engineering, can solve the problems of large transmission resistance of catalytic packing, uneven distribution of vapor and liquid, etc., and achieve the effects of improved catalyst efficiency, uniform liquid distribution, and excellent catalytic performance

Active Publication Date: 2021-08-03
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This technology can improve the problems of catalytic packing such as large transfer resistance and uneven distribution of vapor and liquid in the existing catalyst package of reactive distillation.

Method used

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  • Preparation method of ceramic surface supported catalytic filler
  • Preparation method of ceramic surface supported catalytic filler
  • Preparation method of ceramic surface supported catalytic filler

Examples

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preparation example Construction

[0029] The preparation method of the present invention comprises the following steps:

[0030] (1) Wash the commercially purchased 3mm ceramic Raschig ring packing with 10% sodium hydroxide solution at 70-85°C for 12h, wash with water until neutral, and dry at 100°C for 24h before use;

[0031] (2) Configure Tris-HCl buffer solution with pH = 8.0-9.0, compound it with absolute ethanol at 3-6:1, soak the Raschig ring obtained in step (1), and add a certain amount of mono Nitric acid, aminosilane, vinylsilane, shake at room temperature for 8-18 hours to hydrolyze and oxidize under weak alkaline conditions, form small balls and deposit on the ceramic surface, and then raise the temperature to 65-80°C to cross-link the small balls to form a coating Layer, after absolute ethanol cleaning, obtains the Raschig ring that the surface has been treated;

[0032] (3) Configure a compound solution of vinylimidazole, cross-linking agent and initiator in a certain proportion, and after stir...

Embodiment 1

[0037] Prepare a compound solution of 30ml Tris-HCl buffer (pH=8.5) + 10ml ethanol in a conical flask, add 30g of Raschigcycline after alkali washing, shake it well, add 100mg of tannic acid, 1.5μL of γ-aminopropyl Triethoxysilane and 3 μL of vinyltriethoxysilane were shaken at room temperature for 18 hours, and then the solution was heated to 75° C. for 3 hours.

[0038] Take 0.68g of vinylimidazole, 0.4g of divinylbenzene, 0.08g of azobisisobutyronitrile, and 5g of treated Raschig rings, mix them evenly, use a circulating water vacuum pump to evacuate, and beat and oscillate on the rubber pad several times. After there are no obvious bubbles in the system, put the Raschig ring into a 50ml autoclave, add 30ml of ethyl acetate, react at 100°C for 24h, and then dry at room temperature for 24h.

[0039] Put the dry Raschig ring into the Erlenmeyer flask, add toluene to completely submerge it, add 1.5g propane sultone, react at 80°C for 24 hours, and then exchange it with 1mol / L ...

Embodiment 2

[0041] Prepare a compound solution of 30ml Tris-HCl buffer (pH=8.5) + 10ml ethanol in a conical flask, add 30g of alkali-washed Raschigcycline, shake well, add 100mg of tannic acid, 1.5μL of γ-aminopropyl Triethoxysilane, 3 μL vinyltriethoxysilane, after shaking at room temperature for 18 hours, the solution was heated to 75°C for 3 hours.

[0042]Take 1.68g of vinylimidazole, 0.6g of divinylbenzene, 0.08g of azobisisobutyronitrile, and 5g of treated Raschig rings and mix them evenly, then use a circulating water vacuum pump to evacuate, and beat and vibrate on the rubber pad several times , after there are no obvious bubbles in the system, put the Raschig ring into a 50ml autoclave, add 30ml ethyl acetate, react at 100°C for 24h, and then dry at room temperature for 24h.

[0043] Put the dry Raschig ring into the Erlenmeyer flask, add toluene to completely immerse it, add 2g of butane sultone, react at 80°C for 24 hours, and then exchange it with 1mol / L sulfuric acid for 24 h...

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Abstract

A preparation method of a ceramic surface supported catalytic filler comprises the following steps of: (1) performing surface treatment on a ceramic Raschig ring filler: washing the filler with alkali and water until the filler is neutral, drying the filler, adding the filler into a compound system of a Tris-HCl buffer solution and absolute ethyl alcohol for infiltration, adding tannic acid, amino silane and vinyl silane, and heating for crosslinking; (2) preparing vinyl imidazole, a cross-linking agent and an initiator, immersing the Raschig ring, knocking and oscillating in a negative pressure state, pre-curing, and putting the Raschig ring and ethyl acetate into a digestion tank for treatment; and (3) introducing a sulfonic acid group into the Raschig ring obtained in the step (2) through quaternization reaction, and exchanging with dilute sulphuric acid to obtain a strongly acidic Raschig ring with catalytic capability. The supported catalytic filler is prepared through in-situ grafting of polyimidazole sulfonate on the surface of ceramic through cooperation of a catechol structure with high adhesiveness and vinyl silane, the catalytic efficiency is high, the defects that a traditional catalyst package is high in mass transfer resistance and the like can be overcome, and the supported catalytic filler has potential application value in the field of reactive distillation.

Description

technical field [0001] The invention relates to the field of applied technologies intersecting materials and chemical engineering, in particular to a method for preparing ceramic surface-loaded catalytic fillers for mass transfer-reaction coupling processes such as reactive distillation. Background technique [0002] As a traditional and effective chemical process intensification technology, reactive distillation has been widely used in the industrial production of reaction systems such as esterification, etherification, and transesterification. Practice has proved that reactive distillation technology has the advantages of shortening the process flow, saving equipment investment, improving product purity, etc., and has high economic benefits. Traditional reactive distillation often uses concentrated sulfuric acid and other liquid acids as catalysts, which will often produce more by-products that affect product purity, and also cause corrosion of equipment and pipelines. Th...

Claims

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Application Information

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IPC IPC(8): B01J31/06C07C67/08C07C67/54C07C69/14B01D3/14C08F8/44C08F226/06C08F212/36
CPCB01J31/069C07C67/08C07C67/54B01D3/14C08F8/44B01J2231/49C07C69/14C08F226/06C08F212/36Y02P20/10
Inventor 沙勇王志伟周道伟张禹
Owner XIAMEN UNIV
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