Preparation method of 6-aminocaproic acid
A technology of aminocaproic acid and hydrochloric acid, which is applied in the field of preparation of 6-aminocaproic acid, can solve the problems of low product purity, achieve high product purity, shorten hydrolysis time, and simple operation
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Embodiment 1)
[0029] The preparation method of the 6-aminocaproic acid of the present embodiment has the following steps:
[0030] ①Add 5.0g caprolactam, 2.1g sodium hydroxide and 25g demineralized water into a 100mL reaction flask, increase the pressure to 0.2MPa, heat up to 120°C, and carry out an alkaline hydrolysis reaction for 1h.
[0031] ② Cool the material after alkaline hydrolysis in step ① to room temperature, and neutralize it with hydrochloric acid with a concentration of 20wt% to pH=7.7±0.1.
[0032] ③ The material after the neutralization treatment in step ② is pressurized through a reverse osmosis device for desalination treatment, and the chloride ion content in the effluent is less than or equal to 10 mg / L as the end point.
[0033] ④ The material after the desalination treatment in step ③ is first decolorized with activated carbon, filtered, the filtrate is concentrated under reduced pressure at 50~65° C. to dryness, ethanol is added while hot, stirred for crystallization,...
Embodiment 2~ Embodiment 9)
[0036] The preparation method of each embodiment is basically the same as that of embodiment 1, and the difference lies in: the temperature, pressure and time of the alkaline hydrolysis reaction, as shown in Table 1 for details.
Embodiment 10~ Embodiment 11)
[0042] The preparation method of each embodiment is basically the same as that of embodiment 1, and the difference lies in: feeding amount, see Table 2 for details.
[0043] Table 2
[0044] Example 1 Example 10 Example 11 Reactor 100mL reaction flask 1L reaction flask 100L Reactor caprolactam 5g 100g 10kg sodium hydroxide 2.1g 42g 4.2kg softened water 25g 500g 50kg weight 5.71g 114.4g 11.35kg yield 98.5% 98.7% 97.9% purity 99.3% 99.1% 99.5%
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