Process for refining caprolactam
A technology of caprolactam and crude caprolactam, which is applied in the field of caprolactam refining technology, can solve the problems of insufficient utilization of ion exchange resin exchange capacity, increased energy consumption in the refining process, and shortened resin regeneration cycle, so as to save costs and resources, and reduce regeneration Frequency, the effect of avoiding waste water
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[0039] Example 1
[0040] The extracted caprolactam aqueous solution is subjected to hydrogenation operation under the action of Raney nickel catalyst to remove unsaturated by-products in caprolactam. The hydrogenation reaction temperature is 75℃, H 2 The pressure is 700kPa, the reaction time is 30min, and the catalyst concentration is about 0.05mg Raney nickel per liter.
[0041] The hydrogenated caprolactam aqueous solution is cooled to 45°C and pumped countercurrently into the ion exchange adsorption device through a pump. The ion exchange device takes the pretreated wet cation resin and wet anion resin in a ratio of 1:2, using anion- Yang-yin (volume ratio 1:1:1) is filled in series. Control the temperature of ion exchange adsorption at 45°C and the residence time at 45 min. Measure the conductivity of the discharged liquid, absorbance at 290nm, volatile alkali content and potassium permanganate absorbance. When the extinction value at 290nm of the discharging liquid reaches...
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[0042] Example 2
[0043] Repeat the method described in Example 1, the difference is: the hydrogenation reaction temperature is 90 ℃, H 2 The pressure is 700kPa, the reaction time is 60min, and the catalyst concentration is about 0.15mg Raney nickel per liter. The quality index results of caprolactam after hydrogenation and ion exchange are shown in Table 2, and the operating period and dynamic adsorption capacity are shown in Table 3.
Example Embodiment
[0044] Example 3
[0045] Repeat the method described in Example 1, the difference is: the temperature of the hydrogenation reaction is 105 ℃, H 2 The pressure is 700kPa, the reaction time is 90min, and the catalyst concentration is about 0.10mg Raney nickel per liter. The quality index results of caprolactam after hydrogenation and ion exchange are shown in Table 2, and the operating period and dynamic adsorption capacity are shown in Table 3.
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