Preparation
2-Hydroxyethylhydrazine is prepared by heating about 2 to 17 parts of hydrazine hydrate dissolved in water to about 30℃ to about 100℃. in a closed system. Then, 1 part of ethylene oxide is gradually added to the hydrazine hydrate, and the temperature of the reaction mixture is maintained in the range of about 30℃ to 70℃ during the addition.
Synthesis
The general procedure for synthesizing 2-hydrazinoethanol from ethylene oxide was as follows: ethylene oxide was added to a VO1 liquefied gas storage tank and pressurized to 1.0~1.5 MPa using nitrogen. 80% hydrazine hydrate was added to a VO2 storage tank, and the molar ratio of hydrazine hydrate to ethylene oxide was controlled to be 8:1. the hydrazine hydrate was fed at a total feed flow rate of 2.0 L/h via feed pumps PO1 and PO2, respectively. The temperature of the micro-mixer was maintained at 40°C, the temperature of the cracking reactor was set at 60°C, the temperature of the micro-heat exchanger was controlled in the range of 0-10°C, and the back pressure of the back-pressure valve was set at 1.5-2.5 MPa. The two liquid feedstocks were mixed in a CPMM-R300 micro-mixer and then entered into the cracking reactor for further reaction. The reaction liquid is cooled by a micro heat exchanger and then micro-fed to the receiving vessel. Most of the water and excess hydrazine hydrate were removed by decompression distillation, and the final colorless oily liquid 2-hydroxyethylhydrazine was obtained. The purity of the product was 89.5% and the yield was 98% by GC. Finally, the entire microreactor system was washed using water.
References
[1] Patent: CN104876833, 2016, B. Location in patent: Paragraph 0037; 0038
[2] Patent: EP2952509, 2015, A1. Location in patent: Paragraph 0041; 0042
[3] Bulletin de la Societe Chimique de France, 1939, vol. <5> 6, p. 708,714
[4] Ukrainskii Khimicheskii Zhurnal (Russian Edition), 1928, vol. 3, p. 125,128
[5] Chem. Zentralbl., 1930, vol. 101, # I, p. 2867
