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

A technology of o-fluoronitrobenzene and o-fluoroaniline, which is applied in the catalyst and preparation field for preparing o-fluoroaniline by hydrogenation of o-fluoronitrobenzene, can solve the problems of less personnel demand, poor safety, less investment, etc., and achieves equipment and Environmental pollution-free, good stability, less dosage

Active Publication Date: 2014-10-29
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 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%.

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

[0031] 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;

[0032] 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%;

[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 solution A dropwise to the suspension B...

Embodiment 2

[0040] 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%.

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

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

[0043] 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%;

[0044] 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;

[0045] Step 4. Add the stirred solution A dropwise to t...

Embodiment 3

[0051] 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%.

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

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

[0054] 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%;

[0055] 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;

[0056] Step 4. Add solution A and suspension B after stirring in step 3, and the sodium carbonate solution with a mass concentr...

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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 specifically relates to a catalyst for preparing o-fluoroaniline by hydrogenation of o-fluoronitrobenzene and a preparation method thereof. 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-...

Claims

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Application Information

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Patent Type & Authority Applications(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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