A method for improving the yield of iminodiacetic acid
A technology of iminodiacetic acid and iminodiacetic acid disodium salt, which is applied in the field of improving the yield of iminodiacetic acid, can solve the problem of increasing the amount of waste water produced and the difficulty of treatment, affecting the yield of iminodiacetic acid, and the number of mother liquor cycles, etc. problem, to achieve the effect of yield increase
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Embodiment 1
[0038] Another iminodiacetonitrile (100g, 95%, 1mol) was hydrolyzed with sodium hydroxide solution (585g, 15%, 2.2mol) at 60-65°C, heated to 100°C after hydrolysis, kept for 1h, and 27.5% hydrogen peroxide was added 3g, keep warm at 100°C for 1h, add 36wt% hydrochloric acid dropwise to neutralize to a pH value of 4.5-5.5, concentrate under reduced pressure and distill 385g of water, heat up to 85°C and filter while hot to obtain the filtrate and filter cake, add 36wt% to the filtrate dropwise % hydrochloric acid to a pH value of 1.8-2.2, cooled to 20°C and kept for 1 hour, filtered, the filter cake was washed with 25mL of water, dried to obtain a solid; The batch data are shown in Table 1.
[0039] Table 1: Preparation of iminodiacetic acid by hydrolysis of iminodiacetonitrile sodium hydroxide and acidification with hydrochloric acid
[0040]
Embodiment 2
[0044] Another iminodiacetonitrile (100g, 95%, 1mol) was hydrolyzed with sodium hydroxide solution (585g, 15%, 2.2mol) at 55-60°C, heated to 105°C after hydrolysis, kept for 1h, and added 27.5% hydrogen peroxide 3g, keep warm at 105°C for 1h, add 93wt% sulfuric acid dropwise to neutralize to a pH of 4.5-5.5, concentrate under reduced pressure and distill 85g of water, heat up to 90°C and filter while hot to obtain filtrate and filter cake, add 93wt% to the filtrate dropwise % sulfuric acid to a pH value of 1.8-2.2, cooled to 20°C and kept for 1 hour, filtered, the filter cake was washed with 25mL water, dried to obtain a solid; The batch data are shown in Table 2.
[0045] Table 2: Preparation of iminodiacetic acid by hydrolysis of iminodiacetonitrile sodium hydroxide and sulfuric acid acidification
[0046]
Embodiment 3
[0050] Another iminodiacetonitrile (100g, 95%, 1mol) was hydrolyzed with sodium hydroxide solution (585g, 15%, 2.2mol) at 60-65°C, heated to 100°C after hydrolysis, kept for 1 hour, and added 35% hydrogen peroxide 2.4g, keep warm at 100°C for 1h, add 36wt% hydrochloric acid dropwise to neutralize to pH 1.8-2.2, cool to 5-10°C, keep warm for 2h, filter to obtain the filtrate and filter cake, and dry the filter cake to obtain the product. Evaporate about 505g of water from the filtrate under reduced pressure, cool to 20°C and keep warm for 1 hour, filter, wash the filter cake with 25mL of water, and apply the filtrate to the next batch for three consecutive batches.
[0051] Table 3: Iminodiacetonitrile sodium hydroxide hydrolysis hydrochloric acid acidification to iminodiacetic acid
[0052]
[0053]
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