Producing long chain amino and dibasic acids
A technology of dodecanedicarboxylic acid and amino acid is applied in the production field of long-chain amino acids and dibasic acids, and achieves the effects of simplifying the separation process, good economy and stable process conditions
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Embodiment 1
[0138] This example concerns the production of 11-aminoundecanoic acid and dodecanedioic acid.
[0139] 90 g of 12-ketostearic acid was mixed with 200 mL of water, and then an aqueous solution (about 8%) containing 14.5 g of hydroxylamine sulfate was added. The mixture was vigorously stirred at 70-85°C while adjusting the pH of the reaction solution with aqueous ammonia and maintaining the pH at 4.5-5.0. The reaction was tracked by HPLC. After 2 hours of reaction, the starting material was completely converted into 12-oximino stearic acid.
[0140] After the oximation reaction is completed, the mixture is allowed to stand for phase separation, the lower water phase is separated, and the upper oil phase is vacuum-dried. The obtained product was dissolved in 500 mL of 98% methanesulfonic acid and heated to 140° C., and the Beckmann rearrangement was completed after 4 hours of reaction. The reaction was quenched by adding 500 mL of water. Filtration and washing with deionized ...
Embodiment 2
[0147] This example relates to the production of 9-aminononanoic acid and sebacic acid.
[0148] 90 g of 10-ketostearic acid was mixed with 200 mL of water, and then an aqueous solution (about 8%) containing 12.5 g of hydroxylamine sulfate was added. The mixture was vigorously stirred at 70-80° C. for 2 h, while adjusting the pH of the reaction solution with aqueous ammonia and maintaining the pH at 4.5-5.0. HPLC followed the reaction, and the starting material was completely converted to 10-oximinostearic acid.
[0149] The water phase was separated, and the oil phase was vacuum-dried and dissolved in a mixture of 100 g of trifluoroacetic acid and 100 g of acetonitrile, and the reaction was heated to reflux for 8 hours to complete the Beckmann rearrangement. After the solvent was recovered by distillation, 300 mL of water was added to precipitate an off-white mixed amide fatty acid product.
[0150] The solid mixed amide fatty acid was dissolved in 200mL of acetic acid, and...
Embodiment 3
[0155] This example concerns the production of 13-aminotridecanoic acid and tetradecanedioic acid.
[0156] 100 g of 14-ketoarachidic acid was mixed with 200 mL of water, and then an aqueous solution (about 8%) containing 16.5 g of hydroxylamine sulfate was added. The mixture was vigorously stirred at 70-85° C. for 2 h, while adjusting the pH value of the reaction solution with aqueous ammonia and maintaining the pH value at 4.5-5.0. The reaction was followed by HPLC, and the starting material was completely converted to 14-oximinoarachidic acid.
[0157] The water phase was separated, and the oil phase was vacuum-dried to obtain a waxy solid. The waxy solid was slowly added to 300 mL of 98% sulfuric acid at 100 °C. After the solution was stirred at 100°C for 2 h, the Beckmann rearrangement was completed, and 800 g of ice was added to quench the reaction. Filter and wash with water to obtain a dark mixed amide fatty acid product.
[0158] Add the mixed amide fatty acid and...
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