Extraction and purification method for binary acid amine salt
A technology of dibasic acid amine salt and acid amine salt, which is applied in the separation/purification of carboxylic acid compounds, purification/separation of amino compounds, organic chemistry, etc., and can solve the problems of high cost, low yield, and high cost of polymerization products
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preparation Embodiment 1
[0096] Preparation of Sebacic Acid Pentylenediamine Salt Fermentation Broth
[0097] 1. Preparation of ammonium sebacate fermentation broth
[0098] 1.1 Strain activation:
[0099] Take the glycerol tube strain of Candida and inoculate it into a seed bottle containing YPD culture. The pH is natural, and cultured on a shaker at 220 rpm at 29°C for 1 day; YPD medium includes: 20g / L glucose, 10g / L yeast extract powder , 20g / l peptone; pH7.0;
[0100] 1.2 Cultivation in seed pots and prepare seed liquid:
[0101] Take the seeds of the seed bottle and insert them into the seed tank containing the seed culture medium. After inoculation, the initial pH value of the fermentation system is 6.0, at 29℃, the ventilation ratio is 0.5vvm, the tank pressure is 0.1MPa, and a certain stirring speed is maintained to control the seeds. Dissolved oxygen in the cultivation process is greater than or equal to 10%, culture for 18-20h, and the standard for culturing mature seeds is that the OD620 is 15 afte...
preparation Embodiment 2
[0112] Preparation of dodecanedioic acid-pentanediamine salt fermentation broth
[0113] 1. Preparation of ammonium dodecanoate fermentation broth
[0114] 1.1 Strain activation:
[0115] Take the glycerol tube strain of Candida and inoculate it in a seed bottle containing YPD culture. The pH is natural, at 29℃, 220rpm, amplitude 26-50mm shaker culture for 1 day; YPD medium includes: 20g / L glucose, 10g / L yeast extract powder, 20g / l peptone; pH7.0-7.5;
[0116] 1.2 Cultivation in seed pot and prepare seed liquid:
[0117] Take the seeds of the seed bottle and insert them into the seed tank containing the seed culture medium. After inoculation, the initial pH value of the fermentation system is 6.0, at 29℃, the ventilation ratio is 0.5vvm, the tank pressure is 0.1MPa, and the stirring speed is maintained to control the seeds. Dissolved oxygen in the culture process is greater than or equal to 10%, culture for 18 hours, and the standard for culturing mature seeds is that the OD620 of 15...
Embodiment 1
[0128] The preparation method of sebacic acid pentanediamine salt includes the following steps:
[0129] (1) Take the pentanediamine sebacate solution prepared in Preparation Example 1, wherein the pentanediamine sebacate salt ( - OOC(CH 2 ) 8 COO -+ H 3 N-(CH 2 ) 5 -NH 3+ The content of) is 15% (mass percentage), the pH value is 7.8, heated at 90°C for 60 minutes, and then centrifuged at 4500 rpm for 5 minutes at 80°C to obtain the supernatant;
[0130] (2) The supernatant liquid obtained in step (1) is rotary steamed and dried to a water content of 1wt% to obtain a solid. The solid is mixed with alcohol and water as a solvent (ethanol: water = 70:1), and the mixture is evenly mixed. The mass ratio of water mixed solvent and dibasic acid amine salt is 1.5:1. Start cooling from 80℃, first reduce the temperature to 30℃ at the rate of 1℃ / 5min, keep it for 1h; then reduce the temperature by 10℃ at the rate of 1℃ / 10min , Incubate for 0.5h to obtain pentanediamine sebacate.
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