Method for preparing o-fluoroaniline by hydrogenating o-fluoronitrobenzene

A technology of o-fluoronitrobenzene and o-fluoroaniline, which is applied in the field of o-fluoroaniline hydrogenation to prepare o-fluoroaniline, can solve the problems of less personnel demand, poor safety, and less investment, and achieve large processing capacity and excellent reaction conditions Mild, highly catalytic effect

Active Publication Date: 2014-11-05
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

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] The catalyst of this embodiment includes Al 2 O 3 Carrier, supported 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%.

[0025] The preparation method of the catalyst includes the following steps:

[0026] Step 1. Dissolve 0.3g platinum chloride with platinum, 0.3g tin chloride with tin, and potassium chloride 0.3g with potassium in dilute nitric acid with a mass concentration of 2% and mix them to obtain solution A;

[0027] Step 2: Add 141.6g pseudo-boehmite (containing 99.1g Al 2 O 3 ) Adding to deionized water to obtain 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%;

[0028] 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;

[0029] Step 4. Add the stirred solution A dropwise to the suspension B...

Embodiment 2

[0035] The catalyst of this embodiment includes Al 2 O 3 Carrier, supported on Al 2 O 3 Pt, Zn and Ag on the carrier; the mass percentage of Pt in the catalyst is 0.5%, the mass percentage of Zn is 0.15%, and the mass percentage of Ag is 0.5%.

[0036] The preparation method of the catalyst includes the following steps:

[0037] Step 1. Dissolve 0.5 g platinum chloride with platinum, 0.15 g zinc nitrate with zinc, and 0.5 g silver nitrate with silver nitrate in dilute nitric acid with a mass concentration of 1% and mix them uniformly to obtain solution A;

[0038] Step 2: Add 141.2g pseudo-boehmite (containing 98.85g Al 2 O 3 ) Adding to deionized water to obtain 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%;

[0039] Step 3: Heat the solution A in step 1 and the suspension solution B in step 2 to 80°C and stir for 1 hour;

[0040] Step 4. Add the stirred solution A dr...

Embodiment 3

[0046] The catalyst of this embodiment includes Al 2 O 3 Carrier, supported 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%.

[0047] The preparation method of the catalyst includes the following steps:

[0048] Step 1. Dissolve 0.5g platinum nitrate with platinum, 0.2g tin chloride with tin and 0.25g cobalt chloride with cobalt in dilute nitric acid with a mass concentration of 3% and mix them uniformly to obtain solution A;

[0049] Step 2: Set the 99.05g specific surface area to 150m 2 / g, nano alumina with an average particle size of 5nm is added to deionized water to obtain suspension B with a mass concentration of 60%;

[0050] Step 3: Heat the solution A in step 1 and the suspension solution B in step 2 to 70°C and stir for 2 hours;

[0051] Step 4. Add the stirred solution A and suspension B in step 3 together with the sodium carbonate solution with a mass conce...

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Abstract

The invention discloses a method for preparing o-fluoroaniline by hydrogenating o-fluoronitrobenzene. The method comprises the following steps: 1, filling a fixed bed reactor with a catalyst, introducing air and heating; 2, uniformly mixing o-fluoronitrobenzene steam and preheated hydrogen to obtain mixed gas, introducing the mixed gas into the fixed bed reactor, and performing a catalytic hydrogenation reaction in the presence of the catalyst; and 3, delivering the material subjected to the catalytic hydrogenation reaction into a condenser, condensing the material to convert the o-fluoronitrobenzene steam in the material into a liquid state, and separating the liquid-state o-fluoronitrobenzene in an oil-water separator to obtain oil-state o-fluoroaniline. The o-fluoronitrobenzene is catalytically hydrogenated by adopting the method, the treatment amount is large, the o-fluoronitrobenzene is completely converted, the molar conversion rate of the o-fluoronitrobenzene is 100 percent, and the molar percentage of a defluorinated product is less than 0.1 percent; and the product separating and purifying operation is simple at low energy consumption, and no toxic or harmful ions are doped in the product.

Description

Technical field [0001] The invention belongs to the technical field of catalytic hydrogenation, and specifically relates to a 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 heat-sensitive dye FH-102, which is a widely used and excellent black heat-sensitive dye. The dye can be used in the production of computer terminal output printing paper, ECG recording paper, telephone fax paper and transparent thermal film for oil fields. At present, the main domestic production of o-fluoroaniline is the reduction of o-fluoronitrobenzene with iron powder. This process will produce a large amount of iron sludge (every 1t of o-fluoroaniline will produce 2.2t~2.4t iron sludge), and it will also A large amount of amine-containing wastewater is produced (8t-10t of amine-containing wastewater ...

Claims

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Application Information

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IPC IPC(8): C07C209/36C07C211/52B01J23/62B01J23/66B01J23/89B01J23/63B01J23/656
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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