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Acidic donut-shaped macroporous/mesoporous material, preparation method thereof, and application of acidic donut-shaped macroporous/mesoporous material in preparation of 2, 6-bis(imino)pyridine

A technology of mesoporous materials and doughnuts, applied in chemical instruments and methods, catalytic reactions, organic compounds/hydrides/coordination complex catalysts, etc., can solve the problems of high reaction temperature, difficult separation of products, and complicated post-processing.

Pending Publication Date: 2021-08-31
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The purpose of the present invention is to overcome the problems of high reaction temperature in the prior art, complex post-treatment, difficult separation of products, etc., to provide a kind of acidic doughnut-shaped macroporous mesoporous material and its preparation method and in the preparation of 2,6-bis Application in (imino)pyridine

Method used

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  • Acidic donut-shaped macroporous/mesoporous material, preparation method thereof, and application of acidic donut-shaped macroporous/mesoporous material in preparation of 2, 6-bis(imino)pyridine
  • Acidic donut-shaped macroporous/mesoporous material, preparation method thereof, and application of acidic donut-shaped macroporous/mesoporous material in preparation of 2, 6-bis(imino)pyridine
  • Acidic donut-shaped macroporous/mesoporous material, preparation method thereof, and application of acidic donut-shaped macroporous/mesoporous material in preparation of 2, 6-bis(imino)pyridine

Examples

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preparation example Construction

[0035] The second aspect of the present invention provides a method for preparing an acidic doughnut-shaped macroporous mesoporous material, wherein the method comprises:

[0036] (1) first contacting the triblock copolymer, N,N-dimethylformamide and hydrochloric acid aqueous solution to obtain a mixed solution;

[0037] (2) Carrying out the second contacting of the mixed solution with tetraethyl orthosilicate, after filtering, washing and drying, the original powder mesoporous material is obtained;

[0038] (3) roasting the raw powder mesoporous material to obtain a doughnut-shaped perforated mesoporous material;

[0039](4) performing thermal activation treatment on the donut-shaped perforated mesoporous material to obtain an activated donut-shaped macroporous mesoporous material;

[0040] (5) Under the protection of nitrogen, acidify the activated donut-shaped macroporous mesoporous material with acetic acid to obtain an acidic donut-shaped perforated mesoporous material. ...

Embodiment 1

[0061] This example is to illustrate the acidic doughnut-shaped macroporous mesoporous material prepared by the method of the present invention.

[0062] (1) Add 2.0 g of P123 and 15 g of N,N-dimethylformamide (DMF) into a solution of 11.2 g of 37% hydrochloric acid and 64 mL of water, and stir at 40°C until P123 is completely dissolved;

[0063] (2) Add 4.45 grams of ethyl orthosilicate to the above solution and stir at 40°C for 24 hours;

[0064] (3) Obtain the original powder mesoporous material after filtering, washing and drying;

[0065] (4) Calcining the raw powder mesoporous material in a muffle furnace at 600°C for 24 hours to remove the template agent to obtain a donut-shaped mesoporous material;

[0066] (5) calcining the doughnut-shaped macroporous mesoporous material under nitrogen protection at 400°C for 10 h (thermal activation), removing hydroxyl groups and residual moisture, and obtaining the donut-shaped macroporous mesoporous material after thermal activati...

Embodiment 2-5

[0075] Prepare acidic donut-shaped macroporous mesoporous material according to the same method as in Example 1, the difference is: the consumption of the triblock copolymer, ethyl tetrasilicate and acetic acid is different, specifically as shown in Table 1, Table 1 is the preparation conditions; and the specific surface area, pore volume, most probable pore diameter and acetic acid content of the prepared mesoporous materials are different, as shown in Table 1, and Table 2 is the MBQ pore structure of donut-shaped macroporous mesoporous materials parameter.

[0076] Table 1

[0077] sample Dosage of P123 (g) P123, ethyl orthosilicate and acetic acid weight ratio Example 1 2.0 1：2.25：0.945 Example 2 2.0 1：2：0.75 Example 3 2.0 1：3：1.33 Example 4 2.0 1：1：0.22 Example 5 2.0 1：2：2

[0078] Table 2

[0079]

[0080]

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Abstract

The invention relates to the field of material preparation, and discloses an acidic donut-shaped macroporous / mesoporous material, a preparation method thereof, and application of the acidic donut-shaped macroporous / mesoporous material in preparation of 2, 6-bis(imino)pyridine. The average particle size of the acidic donut-shaped macroporous / mesoporous material is 3-20 [mu]m, the specific surface area is 200-800 m<2> / g, the pore volume is 1-2 ml / g, and the most probable pore size is 7-10 nm; and acetic acid is attached to the outer surface and / or the inner hole wall of the acidic donut-shaped macroporous / mesoporous material. When the catalyst is applied to an organic reaction, the activity of the catalyst in the organic reaction is far higher than that of industrial p-toluenesulfonic acid, formic acid or acetic acid after catalysis, and the catalyst can be repeatedly used and is more beneficial to environmental protection.

Description

technical field [0001] The present invention relates to material preparation 4, in particular, to an acidic donut-shaped macroporous mesoporous material, its preparation method and its application in the preparation of 2,6-bis(imino)pyridine. Background technique [0002] Mesoporous molecular sieve materials have the advantages of ordered pores, adjustable pore size, large specific surface area and pore volume, and are good catalysts and carrier materials. In recent years, heterogeneous catalysts such as solid acids and heteropolyacids prepared using mesoporous molecular sieve materials as templates not only have high catalytic activity for organic reactions, but also have fewer side reactions and simpler post-treatment. The pore structure of the ordered mesoporous material KIT-6 is similar to that of MCM-48, which is a three-dimensional cubic ordered mesoporous structure, but the pore size of KIT-6 is larger than that of MCM-48, and the pore channels are connected to each o...

Claims

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Application Information

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IPC IPC(8): B01J31/02B01J31/26B01J29/03B01J35/10C07D213/53
CPCB01J31/02B01J31/26B01J29/0308C07D213/53B01J2231/4283B01J35/40B01J35/617B01J35/638B01J35/647B01J35/615
Inventor 亢宇徐向亚刘红梅刘东兵
Owner CHINA PETROLEUM & CHEM CORP
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