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Catalyst for preparing 2-picoline, preparation method and method for preparing 2-picoline therewith

A methylpyridine and catalyst technology, applied in the field of preparing 2-methylpyridine, can solve the problems of high cost of raw materials or catalysts, difficult product separation and purification, low selectivity of target products, etc., and achieves long service life, high selectivity, The effect of less waste

Active Publication Date: 2022-07-12
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Patents CN105218431A and CN109174168A report catalysts for the preparation of 2-picoline by alkylation of pyridine. The yield of 2-picoline can be up to 89.9%, but the price of pyridine is relatively expensive, and the overall economic efficiency of this route is low
[0004] In summary, it can be seen that the technique for synthesizing 2-picoline in the prior art has disadvantages such as low target product selectivity, difficulty in product separation and purification, and high cost of raw materials or catalysts. Therefore, a new method for preparing 2-picoline is developed. Catalysts and a new process route for preparing 2-picoline are of great significance

Method used

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  • Catalyst for preparing 2-picoline, preparation method and method for preparing 2-picoline therewith
  • Catalyst for preparing 2-picoline, preparation method and method for preparing 2-picoline therewith
  • Catalyst for preparing 2-picoline, preparation method and method for preparing 2-picoline therewith

Examples

Experimental program
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Effect test

preparation example Construction

[0033] On the other hand, the described preparation method of the supported palladium catalyst for preparing 2-picoline, comprises the steps:

[0034] i) One or more of praseodymium oxide powder, neodymium oxide powder, erbium oxide powder and ytterbium oxide powder are made into slurry, then shaped and granulated, and calcined at 400-500 ° C for 4-6 hours to obtain a Carrier;

[0035] ii) dissolving the active component precursor (any one in dichlorotetraammine palladium, palladium dichloride, palladium acetate and ammonium tetrachloropalladate) in water to form a solution, adding the auxiliary agent precursor (trichloropalladium); one or more of indium chloride, rhenium trichloride and osmium trichloride) to prepare an impregnating liquid; placing the obtained shaped carrier in the impregnating liquid and stirring evenly, and then stirring at 60-100 °C until all the water evaporates to dryness;

[0036] iii) drying the carrier obtained by impregnation in step ii) at 100-12...

Embodiment 1～10

[0067] Examples 1-10 and their comparative examples 1-3

[0068] The spherical carrier is prepared by a method well known to those skilled in the art, and the specific process is as follows: one or more of praseodymium oxide, neodymium oxide, erbium oxide and ytterbium oxide powder are added into water, stirred to form carrier slurry, and then shaped Granulation, and finally roasting at a temperature of 400-500 ° C for 4-6 hours to obtain a particle size range of 2-5 mm and a BET specific surface area range of 50-150 m 2 / g of spherical carrier. In Comparative Examples 2 to 3, the carrier is a commercial carrier, and the active components and auxiliary agents can be directly impregnated and loaded without forming.

[0069] The supported palladium catalyst is prepared by the impregnation method, and the specific process is as follows: the active component (dichlorotetraammonium palladium, ammonium tetrachloropalladate, palladium acetate or palladium dichloride) and optional au...

Embodiment 11～23 and comparative example 4～6

[0079] Select 13 catalysts from 1# to 10# and D1# to D3# for screening. The method is as follows: use a fixed bed reactor from top to bottom to investigate the catalyst reaction performance. The fixed bed reactor is stainless steel with an inner diameter of 4cm and a length of 80cm. Tube. The catalyst loading was 20 g and diluted to 100 mL with glass beads. Each catalyst was loaded into a fixed bed reactor, and each catalyst was activated under nitrogen protection, and activated at 400° C. for 2 hours. Then it was cooled to below 40°C, and the nitrogen purging was stopped. After mixing acrylonitrile and acetone according to a certain mass ratio, the liquid phase passes through the catalyst bed, and under the condition of continuously feeding hydrogen, the fixed-bed reactor is adjusted to the temperature required for the reaction, and the hydrogen pressure is adjusted to maintain suitable reaction conditions. After 20 hours of stable reaction, the composition of the reaction ...

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Abstract

The present invention provides a catalyst for preparing 2-picoline, a preparation method and a method for preparing 2-picoline by using the same. The catalyst includes an active component, an auxiliary agent and a carrier; the active component is palladium; the auxiliary agent is one or more of indium element, rhenium element and osmium element; the carrier is one or more of praseodymium oxide, neodymium oxide, erbium oxide and ytterbium oxide. The method of the invention converts acetone and acrylonitrile into 2-picoline in one pot under the action of the catalyst, and has the advantages of simple operation process, cheap and readily available raw materials, high yield of the target product, easy separation of the target product, and the like. The problems of low selectivity of target products, difficult product separation and purification, and high cost of raw materials or catalysts existing in the prior art are solved.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and particularly relates to a catalyst for preparing 2-picoline, a preparation method and a method for preparing 2-picoline with the same. Background technique [0002] 2-Methylpyridine is an important organic synthesis intermediate, which has a wide range of applications in the field of fine chemicals. An important raw material-butadiene latex. In addition, 2-methylpyridine can also be used to prepare herbicides, veterinary drugs, nitrogen fertilizer synergists, dye intermediates, pharmaceutical chlorpheniramine, long-acting sulfonamides, etc. [0003] There are three main methods for preparing 2-picoline at present: (1) acetaldehyde and liquid ammonia are used as raw materials to synthesize 2-picoline and 4-picoline simultaneously. Patent CN103252254A reports that chromium, lanthanum and platinum modified molecular sieve catalysts are used to catalyze the reaction of liquid ammonia ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/63B01J23/656C07D213/12C07D213/16
CPCB01J23/63B01J23/6567C07D213/12C07D213/16Y02P20/52Y02P20/584
Inventor 沈稳黄文学张永振谢硕孙媛媛马宏宇宋明焱
Owner WANHUA CHEM GRP CO LTD
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