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Catalyst and preparation method for preparing o-fluoroaniline by hydrogenation of o-fluoronitrobenzene

A technology of o-fluoronitrobenzene and o-fluoroaniline, which is applied in the field of catalyst and preparation of o-fluoroaniline by hydrogenation of o-fluoronitrobenzene, can solve the problems of less personnel demand, poor safety, and large manpower, and achieve equipment and No pollution to the environment, good stability and long service life

Active Publication Date: 2016-04-13
XIAN CATALYST NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method requires less initial investment and is easy to implement, but it requires a lot of manpower, has poor safety, and produces a lot of waste liquid and waste residue. It has not yet been industrialized.
At present, there are few literature reports on the method and catalyst for the preparation of o-fluoroaniline by continuous fixed-bed catalytic hydrogenation. This process is safe, environmentally friendly, high in production efficiency, and requires less personnel. It is beneficial to large-scale industrial production in the long run.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] The catalyst of this example includes Al 2 o 3 Carrier, loaded on Al 2 o 3 Pt, Sn and K on the carrier; the mass percentage of Pt in the catalyst is 0.3%, the mass percentage of Sn is 0.3%, and the mass percentage of K is 0.3%.

[0030] The preparation method of catalyst comprises the following steps:

[0031] Step 1, dissolving platinum chloride containing 0.3g of platinum, tin chloride containing 0.3g of tin and potassium chloride containing 0.3g of potassium in dilute nitric acid with a mass concentration of 2% and mixing uniformly to obtain solution A;

[0032] Step 2, 141.6g pseudo-boehmite (containing 99.1gAl 2 o 3 ) into deionized water to obtain a suspension B with a mass concentration of 50%; the specific surface area of ​​the pseudo-boehmite is 250m 2 / g, the mass content of alumina in pseudo-boehmite is 70%;

[0033] Step 3. Heat the solution A in step 1 and the suspension B in step 2 to 75°C and stir for 1.5 hours;

[0034] Step 4. Add the stirred so...

Embodiment 2

[0040] The catalyst of this example includes Al 2 o 3 Carrier, loaded on Al 2 o 3 Pt, Zn and Ag on the carrier; the mass percentage content of Pt in the catalyst is 0.5%, the mass percentage content of Zn is 0.15%, and the mass percentage content of Ag is 0.5%.

[0041] The preparation method of catalyst comprises the following steps:

[0042] Step 1, dissolving platinum chloride containing 0.5g of platinum, zinc nitrate containing 0.15g of zinc and silver nitrate containing 0.5g of silver in dilute nitric acid with a mass concentration of 1% and mixing uniformly to obtain solution A;

[0043] Step 2, 141.2g pseudo-boehmite (containing 98.85gAl 2 o 3 ) into deionized water to obtain a suspension B with a mass concentration of 40%; the specific surface area of ​​the pseudo-boehmite is 250m 2 / g, the mass content of alumina in pseudo-boehmite is 70%;

[0044] Step 3. Heat the solution A in step 1 and the suspension B in step 2 to 80°C and stir for 1 hour;

[0045] Step 4...

Embodiment 3

[0051] The catalyst of this example includes Al 2 o 3 Carrier, loaded on Al 2 o 3 Pt, Sn and Co on the carrier; the mass percentage of Pt in the catalyst is 0.5%, the mass percentage of Sn is 0.2%, and the mass percentage of Co is 0.25%.

[0052] The preparation method of catalyst comprises the following steps:

[0053] Step 1, dissolving platinum nitrate containing 0.5g of platinum, tin chloride containing 0.2g of tin and cobalt chloride containing 0.25g of cobalt in dilute nitric acid with a mass concentration of 3% and mixing uniformly to obtain solution A;

[0054] Step 2, the specific surface area of ​​99.05g is 150m 2 / g, an average particle diameter of 5nm nano-alumina is added to deionized water to obtain a suspension B with a mass concentration of 60%;

[0055] Step 3. Heat the solution A in step 1 and the suspension B in step 2 to 70°C and stir for 2 hours;

[0056] Step 4, add solution A and suspension B stirred in step 3, and sodium carbonate solution with a ...

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Abstract

The invention discloses a catalyst for preparing o-fluoroaniline from o-fluoronitrobenzene by hydrogenation. The catalyst contains an Al2O3 supporter and the following components in percentage by mass: 0.05%-1% of Pt supported on the Al2O3 supporter, 0.05%-3% of metal M1 and 0.01%-3% of metal M2, wherein the metal M1 is Pd, Sn or Zn; the metal M2 is K, Co, Ga, In, Mn, Ag or Ce. Besides, the invention also provides a preparation method of the catalyst. When the catalyst prepared by the preparation method is used for catalyzing o-fluoronitrobenzene hydrogenation, the mole conversion rate of o-fluoronitrobenzene is up to 100%, the mole percentage of a defluorination product is smaller than 0.1%, the amount of o-fluoronitrobenzene treated by the catalyst of unit mass is large, the use amount of the catalyst is small, and the catalyst can be reused after being regenerated.

Description

technical field [0001] The invention belongs to the technical field of catalyst preparation, and in particular relates to a catalyst and a preparation method for preparing o-fluoroaniline by hydrogenating o-fluoronitrobenzene. Background technique [0002] O-fluoroaniline is an important intermediate in the synthesis of fluorine-containing medicines and dyes. O-fluoroaniline can be used to synthesize thermosensitive dye FH-102, which is a kind of thermosensitive dye with wide application and excellent performance in black. The dye can be used in the production of computer terminal output printing paper, electrocardiogram recording paper, telephone fax paper and transparent heat-sensitive film for oil fields. At present, in China, o-fluoroaniline is mainly produced by reducing o-fluoroaniline with iron powder. This process will produce a large amount of iron sludge (every 1 ton of o-fluoroaniline will produce 2.2t~2.4t of iron sludge), and at the same time A large amount of...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/62B01J23/66B01J23/89B01J23/63B01J23/656C07C211/52C07C209/00
Inventor 万克柔林涛程杰张之翔曾永康曾利辉闫琦
Owner XIAN CATALYST NEW MATERIALS CO LTD
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