Production method of nano-attapulgite composite catalyst for 3-methylpyridine preparation

A nano-attapulgite and composite catalyst technology, which is applied in molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of rare applications, low product purity, and difficult separation, and achieve reduction performance Excellent, good adsorption, good pore permeability

Active Publication Date: 2018-05-04
上海磐石矿业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

3-picoline was first isolated from coal tar, but the separation is difficult and the product purity is low. Now it is widely produced by chemical synthesis
It can be seen from the above prior art that the catalyst carrier for preparing 3-picoline is mostly ZSM zeolite molecular sieve. Attapulgite is a kind of porous rare non-metallic mineral raw material, which has a very large specific surface area and ion exchange property, and is often used as It is used as a catalyst carrier, but the application of attapulgite in the preparation of catalysts from 3-picoline is rare

Method used

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  • Production method of nano-attapulgite composite catalyst for 3-methylpyridine preparation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) Add nano-attapulgite raw ore into 1mol / L hydrochloric acid aqueous solution, separate and wash, then wash with 0.1mol / L silver nitrate solution until there is no chloride ion, then heat and boil with distilled water for 30min, and centrifugally wash to obtain acid-modified nano-attapulgite.

[0024] (2) Mix the acid-modified nano-attapulgite and zeolite molecular sieve with a mass ratio of 1:4, add 0.005g / mL aluminum hydroxide aqueous solution, mix well, dry and grind, and calcinate at 950°C 1h, to obtain nano-attapulgite composite carrier.

[0025] (3) The nano-attapulgite composite carrier is added to the silica sol with a particle size of 150-250nm, fully adsorbed, dried and ground to obtain a nano-attapulgite composite catalyst for the preparation of 3-picoline, wherein, The content of silica sol is 0.1 wt%, and the content of alumina is 20 wt%.

Embodiment 2

[0027] (1) Add nano-attapulgite raw ore into 1.5mol / L hydrochloric acid aqueous solution, separate and wash, then wash with 0.2mol / L silver nitrate solution until there is no chloride ion, then heat and boil with distilled water for 60min, and centrifugally wash to obtain acid modified Sexual nano attapulgite.

[0028] (2) Mix acid-modified nano-attapulgite and zeolite molecular sieve with a mass ratio of 1:10, add 0.01g / mL aluminum hydroxide aqueous solution, mix well, dry and grind, and calcinate at 1000°C 2h, the nano-attapulgite composite carrier was obtained.

[0029] (3) The nano-attapulgite composite carrier is added to the silica sol with a particle size of 150-250nm, fully adsorbed, dried and ground to obtain a nano-attapulgite composite catalyst for the preparation of 3-picoline, wherein, The content of silica sol was 1 wt%, and the content of alumina was 35 wt%.

Embodiment 3

[0031] (1) Add nano-attapulgite raw ore into 1.2mol / L hydrochloric acid aqueous solution, separate and wash, then wash with 0.15mol / L silver nitrate solution until there is no chloride ion, then heat and boil with distilled water for 40min, and centrifugally wash to obtain acid modified Sexual nano attapulgite.

[0032] (2) Mix the acid-modified nano-attapulgite and zeolite molecular sieve with a mass ratio of 1:5, add 0.007g / mL aluminum hydroxide aqueous solution, mix well, dry and grind, and calcinate at 970°C After 1.5 hours, the nano-attapulgite composite carrier was obtained.

[0033] (3) The nano-attapulgite composite carrier is added to the silica sol with a particle size of 150-250nm, fully adsorbed, dried and ground to obtain a nano-attapulgite composite catalyst for the preparation of 3-picoline, wherein, The content of silica sol is 0.5 wt%, and the content of alumina is 25 wt%.

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Abstract

The invention provides a production method of a nano-attapulgite composite catalyst for 3-methylpyridine preparation. The method comprises following steps: nano-attapulgite raw ore is added to an aqueous hydrochloric acid solution for separating and washing, then a silver nitrate solution is utilized for washing, a mixed solution is heated and boiled by distilled water, centrifugal washing is performed, and acid modified nano-attapulgite is obtained; the acid modified nano-attapulgite is mixed uniformly with zeolite molecular sieves, a mixture is added to an aqueous aluminium hydroxide solution and mixed uniformly, a mixed solution is dried, ground and calcined at high temperature, and nano-attapulgite composite supports are obtained; the nano-attapulgite composite supports are added to silicon dioxide sol, sufficient adsorption, drying and grinding are performed, and the nano-attapulgite composite catalyst for the 3-methylpyridine preparation is obtained. According to the prepared catalyst, the zeolite molecular sieves and attapulgite are taken as the composite supports, and aluminium oxide and silicon dioxide are adsorbed into multi-stage support pores, so that catalyst is high in strength, low in cost and good in dispersibility and has good selectivity and high product yield in the 3-methylpyridine preparation.

Description

technical field [0001] The invention belongs to the field of medicinal chemistry, and in particular relates to a production method of a nano-attapulgite composite catalyst used for the preparation of 3-picoline. Background technique [0002] 3-picoline, also known as β-picoline, 3-picoline, is an important pyridine derivative. After a series of reactions, a variety of important fine organic synthesis intermediates can be synthesized, mainly used for the synthesis of nicotinic acid and nicotinamide, which are in great demand in the feed, pharmaceutical and food industries. 3-Methylpyridine was first isolated from coal tar, but the separation is difficult and the product has low purity. Now it is widely produced by chemical synthesis. At present, 3-picoline is mainly obtained by chemical synthesis, and the methods include acrolein ammoniation method, ethanol-formaldehyde ammoniation method, acetaldehyde-formaldehyde ammoniation method, 2-methylpentamethylenediamine method and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/06C07D213/16C07D213/09
CPCB01J29/06B01J2229/186C07D213/09C07D213/16
Inventor 李晓明
Owner 上海磐石矿业有限公司
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