A kind of preparation method and application of palladium/silver alloy nano catalyst

An alloy catalyst and silver nanotechnology, applied in the field of nanocatalyst research, can solve the problems of reducing product purity and producing by-products, and achieve the effects of avoiding by-products, no three wastes, and stable performance

Active Publication Date: 2020-06-09
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The commercial Raney nickel catalyst not only catalyzes the hydrogenation of nitro group to amino group, but also catalyzes the hydrogenation of benzene ring, resulting in the generation of by-products, which reduces the purity of the product

Method used

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  • A kind of preparation method and application of palladium/silver alloy nano catalyst
  • A kind of preparation method and application of palladium/silver alloy nano catalyst
  • A kind of preparation method and application of palladium/silver alloy nano catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 1. Preparation of catalyst:

[0023] Using palladium nitrate and silver nitrate as raw materials and ascorbic acid as reducing agent, palladium / silver alloy nano-catalysts are prepared in the presence of organic modifiers.

[0024] When palladium, silver molar ratio is 0.03:1, palladium / silver alloy nanocatalyst (Pd 0.03 Ag) preparation: respectively weigh 0.0799g of Pd (NO 3 ) 2 2H 2 O, 1.6987g of AgNO 3 and 0.1779g of KH570 silane coupling agent were dissolved in 40mL, 70mL and 10mL of anhydrous ethanol respectively by ultra-dispersion, and stirred and mixed at 50°C for 20min. Use 1.0mol / L NaOH ethanol solution to adjust the pH to 10, add 0.65mol / L ascorbic acid absolute ethanol solution dropwise to the above reaction solution, react at 70°C for 6h, the product is washed with alcohol several times, vacuum After drying, the Pd 0.03 Ag alloy nanocatalysts.

[0025] 2.1-Nitroanthraquinone selective catalytic hydrogenation to prepare 1-aminoanthraquinone reaction: ...

Embodiment 2

[0028] Same as in Example 1, only changing the amount of catalyst: 0.01g, 0.02g, 0.04g, 0.06g, 0.1g, to carry out selective hydrogenation reaction of 1-nitroanthraquinone. The product selectivity and raw material conversion rate obtained are shown in Table 1.

[0029] Table 1 at 1.0MPa H 2 The reaction temperature is 110°C, and the reaction time is 4 hours under heat preservation. When the amount of catalyst is different, the selectivity of the palladium / silver alloy nanocatalyst to catalyze the hydrogenation reaction of 1-nitroanthraquinone to produce 1-aminoanthraquinone and the conversion rate of raw materials

[0030]

Embodiment 3

[0032] Same as in Example 1, only changing the temperature of the reactor to 80°C, 90°C, 110°C, 130°C, 140°C to carry out the selective hydrogenation reaction of 1-nitroanthraquinone. The resulting product selectivity and feedstock conversion are shown in Table 2.

[0033] Table 2 at 1.0MPa H 2 Under pressure, when the amount of catalyst is 0.06g, under different reaction temperatures, under heat preservation for 4 hours, the palladium / silver alloy nano-catalyst selectively catalyzes the selectivity of 1-aminoanthraquinone hydrogenation reaction product 1-aminoanthraquinone and the conversion of raw materials Rate

[0034]

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Abstract

The invention provides a preparation method and application of a palladium / silver alloy nanocatalyst. The preparation method comprises the following steps: weighing a certain amount of Pd and Ag metal precursors, dissolving the Pd and Ag metal precursors into an absolute ethanol solution respectively, stirring, mixing, adding an alcohol solution of an organic modifier, mixing and stirring for 20 min at 30-60 DEG C, adjusting the pH value of a reaction solution with an ethanol solution of NaOH, raising the temperature to 70 DEG C, dropwise adding an ethanol solution of hydrazine hydrate / ascorbic acid with a certain concentration into the reaction solution, reacting for 4-8 h, washing for multiple times with absolute ethanol, and performing vacuum drying to obtain the palladium / silver alloy nanocatalyst. The palladium / silver alloy nanocatalyst prepared by the preparation method provided by the invention is applied to a reaction for preparing 1-aminoanthraquinone through catalytic hydrogenation of 1-nitroanthraquinone, and shows high catalytic activity and stability; in addition, by a method for preparing 1-aminoanthraquinone by using the palladium / silver alloy nanocatalyst, a process requirement is simple, the using amount of the catalyst is small, environment friendliness is achieved, and industrial requirements are met.

Description

technical field [0001] The invention relates to a preparation method and application of a palladium / silver alloy nano-catalyst and belongs to the field of nano-catalyst research. Background technique [0002] 1-Aminoanthraquinone is mainly used in the production of anthraquinone dyes, such as bromic acid, acid blue 78, disperse red RLZ, disperse brilliant red (E-RLN, FB), reduced olive (T, B, 5G), reduced Raw materials for gray M, reactive brilliant blue (X-BR, KN-R), etc. 1-Aminoanthraquinone can also be used in the production of inks, coatings and pigments. In recent years, it has also been used as a photosensitizer for liquid crystal dyes and photodegradable polyesters. With the development of my country's dye industry, the demand for 1-aminoanthraquinone is very large. In 2014, the domestic demand for anthraquinone dyes exceeded 8,000 tons, and it increased year by year with a growth rate of 15%-20%. The domestic market is very broad; The preparation of 1-aminoanthraqui...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/50C07C221/00C07C225/34
CPCB01J23/50C07C221/00C07C225/34
Inventor 杨晨晨王爱丽殷恒波
Owner JIANGSU UNIV
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