Water → Nitric Acid

HRID 1375259Notes

Reaction equation

HRID 1375259 reaction equation
[CH:1]1[CH:6]=[CH:5][C:4]([NH:7][N:8]=[C:9]2[C:14](=[O:15])[C:13]3[C:16]([NH2:31])=[C:17]([N:20]=[N:21][C:22]4[CH:27]=[CH:26][C:25]([N+:28]([O-:30])=[O:29])=[CH:24][CH:23]=4)[CH:18]=[CH:19][C:12]=3[CH:11]=[CH:10]2)=[CH:3][CH:2]=1.[OH2:32]>>[N+:28]([O-:30])([OH:32])=[O:29].[CH:1]1[CH:6]=[CH:5][C:4]([NH:7][N:8]=[C:9]2[C:14](=[O:15])[C:13]3[C:16]([NH2:31])=[C:17]([N:20]=[N:21][C:22]4[CH:27]=[CH:26][C:25]([N+:28]([O-:30])=[O:29])=[CH:24][CH:23]=4)[CH:18]=[CH:19][C:12]=3[CH:11]=[CH:10]2)=[CH:3][CH:2]=1

Participants

4

Reactant 2

HCID 962Water2×HCID 178508065HCID 178508065, compound3×

Product 2

HCID 944Nitric AcidYield 10%HCID 178508065HCID 178508065, compound

Procedure

The preparation of the Levanyl Black involves rolling 5 g of Levanyl Black in about 572 g of water and the preparation of the Nigrosin Black involves rolling 2–3 g of the Nigrosin Black in about 420 g of water. The Nigrosin Black solution should have a pH of 3.0–6.0 which can be obtained with the addition of an appropriate quantity of 10% nitric acid after the Nigrosin Black is rolled. In this example, the order of ingredients is particularly important for obtaining a stable formulation. Experiments have shown that an intermediate silicate formulation should be made in a separate vessel by first adding the acid to about 20 g of water followed by the addition of the alcohol and organic silicate. Next, the contents of the separate vessel should be shaken to hydrolyze the organic silicate, thereby creating the intermediate silicate formulation. The solvent and remaining water should then be mixed into the separate vessel, thereby making a diluted intermediate silicate formulation. The general conclusion is that it is best to dilute the intermediate formulation with a slow evaporating organic solvent such as 1-propanol and water. The reason is that the final formulation will flash-off more slowly during application and, in turn, provide a glossier finish.

Workup

  1. customThe preparation of the Levanyl Black

Sources & evidence

ORD record
ord-c1c206c676d54ab08387d6527652b14b
Source dataset
uspto-grants-2007_01
Patent number
US07166957B2

Reaction notes

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