Diethylenetriaminepenta(methylene-phosphonic acid) synthesis

Yield:15827-60-8 98.3%

Reaction Conditions:

with hydrogenchloride;phosphonic Acid in water at 115; for 2 h;Large scale;

Steps:

1; 2; 1; 2 Example 1
2813Kg mass of 71.25% phosphorous acid aqueous solution and 2250Kg mass of 31.50% hydrochloric acid were sequentially added to the reaction kettle,Turn on the stirring and exhaust gas recovery device,Then, 500.0Kg of diethylenetriamine was slowly added dropwise to the reaction kettle, and the temperature in the kettle was controlled below 50 ° C. After the neutralization reaction was completed, the temperature in the reactor was maintained at 115 ± 2 ° C by heating up.Set and automatically control the acceleration of formaldehyde dripping: 250Kg / h dripping for 0.5 hour, 500Kg / h dripping for 0.5 hour, and 1000Kg / h dropping to the end of the first stage.A total of 1573Kg of a 40.73% formaldehyde aqueous solution was added dropwise,After holding at 115 ± 2 for 1 hour, the mixture was evaporated to near dryness under atmospheric pressure and then under negative pressure.Stop the negative pressure and add 225Kg hydrochloric acid to the system to control the system temperature to 115 ± 2 .A total of 393Kg of the remaining formaldehyde aqueous solution was added dropwise at a flow rate of 200Kg / h. After holding for 0.5 hours, it was evaporated under negative pressure until no material was taken out from the system.The acidity of hydrochloric acid was adjusted to obtain 5417.6 kg of a brown-yellow transparent DTPMPA aqueous solution with an activity of 50.47%, the yield (calculated as diethylenetriamine) was 98.30%, and the content of by-product hydroxymethylphosphonic acid was 0.74%.

References:

Shandong Taihe Water Treatment Technology Co., Ltd.;Cheng Zhongfa;Lin Xuezhou;Qi Xiaojing;Song Mengmeng;Zhou Xiang;Liu Quanhua CN110804071, 2020, A Location in patent:Paragraph 0018-0021

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