Separation and purification method of 2-nitroethanol
AssigneeFudan University
InventorsFener Chen, Minjie Liu
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Abstract
A separation and purification method of 2-nitroethanol, including: (a) reacting paraformaldehyde with nitromethane in the presence of a base to obtain a mixture of 2-nitroethanol (I), 2-nitro-1,3-propanediol (II) and tris(hydroxymethyl) nitromethane (III); and (b) selecting an extraction solvent in which 2-nitroethanol (I), 2-nitro-1,3-propanediol (II) and tris(hydroxymethyl) nitromethane (III) are different in solubility; adding the extraction solvent to the mixture followed by extraction, separation, and vacuum concentration to obtain the 2-nitroethanol (I).
Claims6
A separation and purification method of 2-nitroethanol (I), comprising:
- (a) reacting paraformaldehyde with nitromethane under the catalysis of a base to obtain a mixture of 2-nitroethanol (I), 2-nitro-1,3-propanediol (II) and tris(hydroxymethyl) nitromethane (III), as shown in the following reaction scheme:
- and
- (b) selecting an extraction solvent in which the 2-nitroethanol (I), 2-nitro-1,3-propanediol (II) and tris(hydroxymethyl) nitromethane (III) are different in solubility;
- adding the extraction solvent to the mixture followed by extraction, separation, and vacuum concentration to obtain the 2-nitroethanol (I);
- wherein the extraction solvent is one or more of C3˜C9 aliphatic esters;
- a mass ratio of the extraction solvent to the paraformaldehyde is (1˜10):
- 1;
- the extraction is performed at −20˜60° C. in a kettle equipment or a continuous extraction equipment;
- and
- the vacuum concentration is performed under a vacuum degree of 0.1˜10 mmHg at 0˜60° C.
Dependencies are inferred from the claim text.