Method for preparing 6-aminocaproic acid
An aminocaproic acid and benchmark technology, applied in the chemical industry, can solve problems such as the inability to apply caprolactam waste liquid, and achieve the effect of solving adverse effects and high purity
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[0032] The preparation method of 6-aminocaproic acid in the present disclosure can extract the effective substances in the waste liquid of caprolactam produced by the rearrangement method, and synthesize the substances into 6-aminocaproic acid. Specifically, in the present disclosure, organic acid is added to the waste liquid of caprolactam produced by the rearrangement method, and the reflux reaction is carried out to convert the caprolactam, aminocaproic acid and caprolactam oligomers in the waste liquid into aminocaproic acid acetate; the first product After dehydration under reduced pressure, add it to an alcohol solvent for dissolution and filter to obtain the first filtrate, which can remove ammonium sulfate in the system, and the first filtrate is mainly the alcohol solution of aminocaproic acid acetate; add the first filtrate to Organic amine or ammonia gas is introduced to adjust the pH to 7-8, and the crude aminocaproic acid is obtained by filtration. The disclosed m...
Embodiment 1
[0048] Take 200g of caprolactam waste liquid, add 35mL of formic acid to carry out reflux reaction to obtain the first product; then dehydrate the first product to near dryness under reduced pressure, and then add 160mL of ethanol to dissolve it to obtain the second product; filter the second product to obtain ammonium sulfate, etc. Inorganic salts and first filtrate. Slowly add 20 g of triethylamine to the first filtrate, and filter to obtain 20 g of crude aminocaproic acid.
[0049] Wherein, the conditions of the reflux reaction include: reacting at 100° C. for 8 hours under total reflux conditions; the conditions of dehydration under reduced pressure include: the pressure is -0.1 MPa, the temperature is 60° C., and the time is 4 hours.
Embodiment 2
[0051] Take 200g of caprolactam waste liquid, add 30mL of acetic acid to carry out reflux reaction to obtain the first product; then dehydrate the first product to near dryness under reduced pressure, and then add 300mL of methanol to dissolve it to obtain the second product; filter the second product to obtain ammonium sulfate, etc. Inorganic salts and first filtrate. Slowly add 30 g of ethylenediamine to the first filtrate, and filter to obtain 24 g of crude aminocaproic acid.
[0052] Wherein, the conditions of the reflux reaction include: reacting at 120° C. for 5 hours under total reflux conditions; the conditions of dehydration under reduced pressure include: the pressure is -0.2 MPa, the temperature is 55° C., and the time is 2 hours.
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