Catalyst for preparing 2-methylpyridine, preparation method and method for preparing 2-methylpyridine by using catalyst

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, low selectivity of target products, difficulty in product separation and purification, etc., and achieves long service life, high selectivity, Simple effect of product separation

Active Publication Date: 2021-08-27
WANHUA CHEM GRP CO LTD
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  • 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-methylpyridine, preparation method and method for preparing 2-methylpyridine by using catalyst
  • Catalyst for preparing 2-methylpyridine, preparation method and method for preparing 2-methylpyridine by using catalyst
  • Catalyst for preparing 2-methylpyridine, preparation method and method for preparing 2-methylpyridine by using catalyst

Examples

Experimental program
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preparation example Construction

[0033] On the other hand, the 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 is made into a slurry, then shaped and granulated, and fired at 400-500°C for 4-6 hours to obtain the formed Carrier;

[0035] ii) The active component precursor (any one of palladium dichlorotetraammine, palladium dichloride, palladium acetate and ammonium tetrachloropalladate) is dissolved in water to form a solution, and the auxiliary agent precursor (trichloro One or more of indium, rhenium trichloride and osmium trichloride) to prepare an impregnation solution; place the obtained molded carrier in the impregnation solution and stir evenly, and then stir at 60-100°C until all the water evaporates;

[0036] iii) drying the support obtained in step ii) by drying at 100-120° C. for 4-6 hours, and then calcining at 400-500...

Embodiment 1～10

[0067] Embodiment 1~10 and its comparative example 1-3

[0068] The spherical carrier is prepared by a method well known to those skilled in the art. The specific process is as follows: add one or more of praseodymium oxide, neodymium oxide, erbium oxide and ytterbium oxide powder into water, stir evenly to form a carrier slurry, and then shape Granulate, and finally bake at 400-500°C for 4-6 hours to obtain a particle size range of 2-5mm and a BET specific surface area range of 50-150m 2 / g spherical carrier. In Comparative Examples 2 to 3, the carrier is a commercial carrier, which does not need to be molded, and the active components and additives can be directly impregnated and loaded.

[0069] Adopt impregnation method to prepare described loaded palladium catalyst, specific process is as follows: Active component (dichloro tetraammine palladium, tetrachloro palladium ammonium, palladium acetate or palladium dichloride) and optional auxiliary agent (for example, three O...

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: use a fixed-bed reactor from top to bottom to investigate the reaction performance of the catalyst. The fixed-bed reactor is a 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 respectively, and each catalyst was activated under the protection of nitrogen, and activated at 400°C for 2 hours. Then cool to below 40°C and stop nitrogen purging. Mix acrylonitrile and acetone according to a certain mass ratio and pass through the catalyst bed in liquid phase. Under the condition of continuously feeding hydrogen, adjust the fixed bed reactor to the temperature required for the reaction, and adjust the hydrogen pressure to maintain suitable reaction conditions. After 20 hours of stable reaction, the composition of the reaction solution was analyzed by gas...

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Abstract

The invention provides a catalyst for preparing 2-methylpyridine, a preparation method of the catalyst and a method for preparing 2-methylpyridine by using the catalyst. The catalyst comprises 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. According to the method, acetone and acrylonitrile are converted into 2-methylpyridine in one pot under the action of the catalyst, and the method has the advantages that the operation process is simple, raw materials are cheap and easy to obtain, the yield of a target product is high, and the target product is easy to separate; the problems of low target product selectivity, difficulty in product separation and purification and high cost of raw materials or catalysts in the prior art are solved.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a catalyst for preparing 2-picoline, a preparation method and a method for preparing 2-picoline with it. Background technique [0002] 2-Methylpyridine is an important intermediate in organic synthesis, which is widely used in the field of fine chemicals, for example, it can be used to prepare 2-vinylpyridine, and the copolymerization of 2-vinylpyridine and butadiene can obtain rubber industry An important raw material - fenfenpyr latex. In addition, 2-picoline can also be used in the preparation of herbicides, veterinary drugs, nitrogen fertilizer synergists, dye intermediates, medicine chlorpheniramine, long-acting sulfonamide, etc. [0003] At present, there are three main methods for preparing 2-picoline: (1) acetaldehyde and liquid ammonia are used as raw materials to simultaneously synthesize 2-picoline and 4-picoline. Patent CN103252254A reports tha...

Claims

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Application Information

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Patent Type & Authority Applications(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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