A kind of powdery pd/sio2 catalyst and its preparation method and application

A catalyst and co-catalyst technology, applied in physical/chemical process catalysts, hydrogenation preparation, chemical instruments and methods, etc., can solve the problems of small specific surface area, poor selectivity, and many side reactions, and achieve high catalytic activity and reduce residence time. Time and less side effects

Active Publication Date: 2016-05-11
SHANDONG NHU PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, with CaCO 3 The supported catalyst is sensitive to acid, strong in alkalinity, has many side reactions such as isomerization and polymerization, high waste rate, small specific surface area, low adsorption and poor selectivity

Method used

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  • A kind of powdery pd/sio2 catalyst and its preparation method and application
  • A kind of powdery pd/sio2 catalyst and its preparation method and application
  • A kind of powdery pd/sio2 catalyst and its preparation method and application

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preparation example Construction

[0061] Catalyst preparation process (1): (1) Submerge 98.15 g of the dried silica gel carrier in an impregnation solution containing 1.00 g of palladium ions, 0.60 g of lead ions, and 0.25 g of chromium ions, and stir and adsorb at 35°C for 2.5 hours , and then vacuum filtration;

[0062] (2) Dry the filter cake obtained in step (1) in a blast drying oven at 55°C, so that the metal precursor is evenly loaded on the inner and outer surfaces of the silica gel carrier;

[0063] (3) The catalyst dried in step (2) is reduced with hydrazine hydrate, and washed with deionized water until it becomes neutral to obtain catalyst A. The preparation methods of catalysts B and C are similar to those of catalyst A, except that the proportions of various active components are different.

[0064] Catalyst preparation process (2): (1) Immerse 90.95g of the silica gel carrier after treatment and drying in the impregnation solution of 5.00g of palladium ions, 3.20g of bismuth ions, and 0.85g of ...

Embodiment 1

[0071] Catalyst A catalyzes the liquid-phase selective hydrogenation of 3-butyn-2-ol in a 2L tank reactor, at a reaction temperature of 20-35°C, a reaction pressure of 2.0MPa, and a catalyst dosage of 1.2% of the mass of acetylenic alcohol After the reaction is complete, the GC analysis results are: the conversion rate of 3-butyn-2-ol in the raw material is 99.9%, and the enol selectivity in the hydrogenation product is 99.6%.

Embodiment 2

[0073] Catalyst B catalyzes the liquid-phase selective hydrogenation of dehydrolinalool in a 2L tank reactor, and the reaction temperature is 25-60°C, the reaction pressure is 2.0MPa, and the volume ratio of ethanol solvent to dehydrolinalool is 1: 1. Under the condition that the amount of catalyst is 1% of the mass of dehydrolinalool, after the reaction is complete, the GC analysis results are: the conversion rate of dehydrolinalool in the raw material is 100%, and the selectivity of linalool in the hydrogenation product is 99.4% %.

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Abstract

The invention discloses a powdered Pd / SiO2 catalyst, which is composed of the following components in percentage by weight: 90-99.98% of silica gel powder, 0.01-5% of a palladium metal component and 0.01-5% of a cocatalyst, wherein the cocatalyst is one or more of lithium, sodium, potassium, chromium, manganese, zinc, silver, titanium, lead and bismuth, and the granularity of the silica gel powder is 150-500 meshes. The catalyst is applied to the hydrogenation reaction of alkynol compounds with a large molecular weight in a reaction kettle, and can eliminate the defects that a currently used lindlar catalyst is strong in alkalinity, more in side effects such as isomerism and polymerization and the like, high in leftovers rate, small in specific surface, low in adsorptivity, poor in selectivity, and the like. The invention also discloses a preparation method of the powdered Pd / SiO2 catalyst and the application of the powdered Pd / SiO2 catalyst in the hydrogenation reaction of alkynol compounds. While the powdered Pd / SiO2 catalyst is applied to the hydrogenation reaction of alkynol compounds so as to produce enol compounds, the powdered Pd / SiO2 catalyst is high in conversion rate and selectivity.

Description

technical field [0001] The invention belongs to the field of supported hydrogenation catalysts, in particular to a powdery Pd / SiO 2 Catalyst and its preparation method and application. Background technique [0002] The selective hydrogenation of acetylenic alcohols to produce enols has important industrial applications, especially in the fields of vitamin and spice preparation. Taking linalool as an example, this compound has high economic value. It can be used as a raw material for the preparation of high-grade spices or essences, and is also an important intermediate for the synthesis of vitamin E and vitamin A. The preparation of linalool from petroleum C5 fraction separation products via 6-methyl-5-hepten-2-one (dehydrolinalool) is an important process route for artificially synthesizing linalool. The main and side reactions of dehydrolinalool to linalool through selective hydrogenation are shown in the following formulas III and IV. The series of hydrogenation side r...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/50B01J23/644B01J23/656B01J23/652C07C29/17C07C33/02C07C33/03
Inventor 马啸陈为超鲁光银张玉忠李耀林
Owner SHANDONG NHU PHARMA
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