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A kind of 2,4-dinitroaniline hydrogenation catalyst and its preparation method and application

A dinitroaniline and hydrogenation catalyst technology, applied in the field of catalysis, can solve the problems of high production cost and selectivity, high loading of catalyst precious metals, non-compliance with environmental protection laws, etc., to achieve large-scale commercial application, Improve the catalytic performance and the effect of not easy to lose

Active Publication Date: 2021-08-31
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the chemical reduction method is used, and under certain conditions, the yield is close to 90%, but there are serious three wastes problems, which do not meet the national environmental protection law; the catalytic hydrogenation method is used, under certain hydrogenation conditions, when the conversion rate is high, the selectivity Low, and the selectivity is lower than 85%, the precious metal loading of each of the catalysts is high, and the production cost and selectivity need to be improved

Method used

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  • A kind of 2,4-dinitroaniline hydrogenation catalyst and its preparation method and application
  • A kind of 2,4-dinitroaniline hydrogenation catalyst and its preparation method and application
  • A kind of 2,4-dinitroaniline hydrogenation catalyst and its preparation method and application

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Experimental program
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Effect test

Embodiment 1

[0027] The preparation steps of catalyst are as follows:

[0028] (1) Take 0.194g SnCl 4 ·5H 2 O was dissolved in a mixed solvent consisting of 40 mL of ultrapure water and 10 mL of ethanol, and then 1.5 g of γ-Al was added as a carrier 2 o 3Stir at 25°C for 15h, wash the obtained solid three times with ethanol and deionized water successively after suction filtration, each time with 30mL washing solution, and then dry at 60°C for 8h, and dry the dried solid in 75% H 2 / N 2 Roasting in a mixed gas, the calcination temperature is 600°C, the calcination time is 3h, and the Sn / γ-Al with a mass percentage of 4.4% is obtained 2 o 3 ;

[0029] (2) Take 0.77mL of RuCl with a concentration of 0.01g / mL 3 Solution and 15mg PVP-K30 were added to a mixed solution consisting of 3.5mL formaldehyde solution, 21mL ethanol and 3.5mL ultrapure water, and the pH value of the mixed solution was adjusted to 7 with 0.025g / mL NaOH aqueous solution, and then 1.25g was added Sn / γ-Al prepared i...

Embodiment 2

[0034] The preparation of the catalyst is similar to Example 1, except that the SnCl 4 ·5H 2 O to ZnCl 2 The amount used is 0.138g, and the rest of the conditions are the same to obtain 0.2%Ru-Al-0.1%RuO 2 -4.4% Zn / γ-Al 2 o 3 Catalyst, evaluation condition is with reference to embodiment 1, and evaluation result is shown in Table 1.

Embodiment 3

[0036] The preparation of the catalyst is similar to Example 1, except that the SnCl 4 ·5H 2 O to CeCl 3 ·7H 2 The amount of O is 0.176g, and the rest of the conditions are the same to obtain 0.2%Ru-Al-0.1%RuO 2 -4.4% Ce / γ-Al 2 o 3 Catalyst, evaluation condition is with reference to embodiment 1, and evaluation result is shown in Table 1.

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Abstract

The invention discloses a 2,4-dinitroaniline hydrogenation catalyst and its preparation method and application. The catalyst is made of Ru-Al alloy and RuO 2 It is the active center and contains metal promoter M, and the general chemical formula can be expressed as Ru‑Al‑RuO 2 ‑M / carrier, where M is one or more of Zn, Sn, Ce, Fe, Cu, Co or Ni, and the carrier is HZSM‑35, Hβ, SBA‑15, γ‑Al 2 o 3 , α‑Al 2 o 3 , SiO 2 、TiO 2 , ZrO 2 or a combination of one or several kinds of activated carbon, the weight ratio of Ru in the catalyst composition is 0.05% to 1%, the weight ratio of Al is 0.2% to 4%, and the weight ratio of M is 0% to 7.5% , the balance is carrier, and Ru and RuO 2 The molar ratio is 1:1~4:1. The preparation process of the catalyst is simple: the precursor salt containing M is first dissolved and then added to the carrier to obtain the M / carrier, and then the active component Ru and the active component Al are sequentially loaded. The catalyst provided by the invention has small load of noble metal, low cost, mild hydrogenation condition, conversion rate up to 100%, and selectivity up to 87%.

Description

technical field [0001] The invention belongs to the technical field of catalysis, and in particular relates to a 2,4-dinitroaniline hydrogenation catalyst and a preparation method and application thereof. Background technique [0002] 4-Nitro-o-phenylenediamine, molecular formula C 6 h 7 N 3 o 2 , is dark red needle-like crystal, with toxicity, soluble in ethanol, acetone and hydrochloric acid solution, insoluble in water. 4-Nitro-o-phenylenediamine is an important organic intermediate, mainly used in the fields of organic synthesis, pigments, dyes, medicines, pesticides, rubber additives, resins and photosensitive materials, and can also be used in the synthesis of α-keto acids and Used as a reagent for the detection of selenium. As an important organic intermediate, 4-nitro-o-phenylenediamine has an increasing market demand, so it is very important to design an economical and environmentally friendly production method. [0003] The production methods of 4-nitro-o-phe...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/60B01J23/62B01J23/63B01J23/89B01J29/67B01J29/74B01J29/03C07C209/36C07C211/52
CPCB01J23/60B01J23/626B01J23/63B01J23/8906B01J23/8913B01J23/892B01J23/8926B01J29/0325B01J29/67B01J29/7415C07C209/36C07C211/52
Inventor 郑进保胡程陈秉辉车黎明张诺伟谢建榕
Owner XIAMEN UNIV