Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

A method for preparing o-fluoroaniline by hydrogenation of o-fluoronitrobenzene

A technology for o-fluoronitrobenzene and o-fluoroaniline, which is applied in the field of preparing o-fluoroaniline by hydrogenation of o-fluoronitrobenzene, can solve the problems of low demand for personnel, poor safety, large manpower and the like, and achieves large processing capacity and reaction conditions. Mild, high catalytic activity

Active Publication Date: 2016-03-23
XIAN CATALYST NEW MATERIALS CO LTD
View PDF3 Cites 0 Cited by
  • 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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 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%.

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

[0026] 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;

[0027] 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%;

[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 so...

Embodiment 2

[0035] 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%.

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

[0037] 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;

[0038] 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%;

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

[0040]Step 4....

Embodiment 3

[0046] 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%.

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

[0048] 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;

[0049] 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%;

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

[0051] Step 4, add solution A and suspension B stirred in step 3, and sodium carbonate solution with a ...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
specific surface areaaaaaaaaaaa
specific surface areaaaaaaaaaaa
specific surface areaaaaaaaaaaa
Login to View More

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 in particular 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 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 amine-containing wastew...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
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
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products