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Process for the Synthesis of N-phosphonomethyliminodiacetic Acid from Iminodiacetonitrile

Author: WangChenJie
Tutor: ZouGang；BiQiang
School: East China University of Science and Technology
Course: Pharmaceutical Engineering
Keywords: Iminodiacetonitrile Iminodiacetic acid PMIDA Synthesis process
CLC: TQ457.29
Type: Master's thesis
Year: 2011
Downloads: 76
Quote: 0
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Abstract


This paper studies the starting material to iminodiacetonitrile hydrolysis of imino diacetic acid , then under the new conditions sulfate media to synthetic production PMIDA process . It mainly consists of three parts: the hydrolysis of iminodiacetonitrile , iminodiacetic acid crystallization and PMIDA synthesis process . Experimental study and optimization of small test process is completed and amplification test pilot and production gradually adjust , and eventually developed into a stable PMIDA Industrial Production . First , iminodiacetonitrile followed by hydrolysis under alkaline conditions acidified with hydrochloric acid to generate the iminodiacetic acid , monosodium salt . Hydrolysis process in materials iminodiacetonitrile ratio, hydrolysis time, hydrolysis temperature were optimized , and try to enlarge the industrial pilot production to determine the optimum conditions : iminodiacetonitrile : sodium hydroxide = 1:2.2 ( moles) and slow addition , the hydrolysis temperature is 42 ° C ± 1 ° C . In this under optimal conditions , the large production iminodiacetonitrile hydrolysis yield of 97.3% . Iminodiacetic acid crystallization process conditions for a sodium salt of the di-acetic acid per mole of amino 1.05-1.1 molar hydrochloric acid was added dropwise , controlled crystallization solution was a pH of 2.2-2.5 . Applying the results showed that the mother liquor of the rung applied is feasible in the production of the crystallization mother liquor rung . The iminodiacetic acid production in the mother liquor to apply three times crystallized fully meet the subsequent synthesis requires PMIDA , large-scale production yield of 93.6% . The sulfuric acid medium at 115 ℃ to iminodiacetic acid with phosphorous acid mixture uniform dropwise addition of formaldehyde, and incubated for 2 hours after the end of the addition synthesis PMIDA . Small test of optimal feeding molar ratio of iminodiacetic acid : phosphorous acid : formaldehyde : = 1:1.2:1.3 , feeding mother liquor apply process than instead of iminodiacetic acid : phosphorous acid : formaldehyde : = 1:1.1 : 1.25. The process verified by the pilot and large-scale production test ( 1,500 kg) , the large-scale production yield of 96.3% . Using the above process from iminodiacetonitrile condensation with formaldehyde and phosphorous acid by alkaline hydrolysis and sulfuric acid medium of industrial production test PMIDA total yield of 87.7% , wastewater emissions only hydrochloric acid medium quarters of the process route one .

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