SU568635A1 - Method of obtaining sodium salt of 4-sulphur acid of 2 amino-1-methyloctadecilaniline - Google Patents

Description

steel, with a height of 250 mm and a diameter of 20 mm, is loaded with 64.8 g (30 ml) of a catalyst of the composition Ni, Cr, Ti, Fe, Zn, Al with an appropriate ratio, eating components 39: 2: 3: 5: 1: 50, leached. At 30 ° C with 20% sodium hydroxide solution at 10% by weight of aluminum. Nitro-blue-2 is dissolved in methanol and fed into the reactor through a metering pump

The process is carried out with a hydrogen pressure of 5 kg / cm and a temperature of 60-80 ° C with a flow rate of 1-4. The proposed method makes it possible to conduct the process, continuously, and shortens the duration of the recovery process.

The table shows the indicators for the process of reduction of nitro-blue-2.

The data in the table show that the proposed process can be carried out at a temperature of 60-80 ° C and a hydrogen pressure of 5 kg / cm, i.e., in milder conditions, and x, than the 3 known methods. The tar of the product, which is unavoidable at high temperatures, is not observed under these conditions. Product analysis was performed by potentiometric titration with 0.1 n. a solution of perchloric acid in acetic acid, as well as, e qualitatively, the color flowed on filter paper during the process. The completeness of the hydrogenation of nitro-blue-2 is carried out

43.9

42.9

40.9

2

2

2

2

2

2

five

2

3

0.1

0.1

0.1 50 50 50

Example 1. A graphite crucible with a capacity of 1 l is loaded with 510 g of aluminum (lOv aluminum. An excess calculated as waste is taken) and placed in a shaft muffle bed. In the molten: And heated to 1100-1200 ° C aluminum brings 409 g of nickel B in the form of shavings or wire. When aluminum interacts with nickel, the temperature rises to IBOO -1900 ° C. At this point, 20 g of chromium, 20 g of titanium, 50 g of iron are introduced into the melt and mixed thoroughly with a quartz rod. When the melt temperature decreases to 1500–1600 ° C, 1 g of zinc is introduced (the addition of ции ка ка др др et.) And the more n-melting temperature of the melt is due to its LOW. As can be seen from the table, the potential of the catalyst corresponds to the potential for complete saturation of the nitro group, i.e., it corresponds to a branded value. The most important advantage of the process is that the catalyst has been operating spontaneously for more than 600 hours of leaching, and loss of activity and stability.

To study the activity and stability in the process of reduction of nitrogolicub-2, catalysts of the following composition were used, wt. %:

34.9

39.9

2

3

2

3 10

five

0.1

0.1 50 50

the melt is stirred and poured into a massive metal mold for rapid cooling. The cooled alloy was crushed to granules of a linear size of 2–5 mm and loaded into a REED: Ktor.

100 ml of crushed 0-weight float; 200 g are loaded into the column reactor between the Daum grids of nickel or stainless

became and the bottom of the pump is fed into the reactor 1 | 0% aqueous solution of caustic soda. The dissolution of lumini in alkali and the formation of a catalytically active surface occur. Leaching depth controlled

by volume of released hydrogen according to the equation.

2BAZA1Oz

2A1 + 6NaOH

The leached catalyst is washed with distilled water from alkali to a neutral reaction with phenolphthalein and dried in a stream of hydrogen to remove moisture. The process of reducing nitro-deep-2 in the form of a 5% methanol solution is carried out on the dried catalyst.

Claims (1)

1. Regulations Dolgoprudny chemical. Skoy Plant for Fine Organic Synthesis, 1962, p. 4-5.