Method for preparing n,n'-bis(2-cyanoethyl)-1,2-ethylenediamine
A cyanoethyl and ethylenediamine technology is applied in the field of preparation for improving the yield of N,N'-bis-1,2-ethylenediamine, and can solve the problems of hindering the commercial application of the preparation method, equipment corrosion and the like, and achieves The effect of saving cost and reducing environmental pollution
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[0013] The preparation method of N,N'-bis(2-cyanoethyl)-1,2-ethylenediamine of the present invention comprises the following steps:
[0014] a. in reactor (for example three-neck round bottom flask), add the alcohol ether based on total reactant weight 10-51.04wt%, preferably the alcohol ether of 30-51.04wt%; More preferably the alcohol ether of 47wt%;
[0015] b. Under stirring, add ethylenediamine into the alcohol ether solution of step a and stir evenly;
[0016] c. At a temperature of 25-70°C, preferably at a temperature of 30-65°C, add acrylonitrile dropwise according to the molar ratio of ethylenediamine to acrylonitrile 1:1.9-2.1 (preferably 1:2.0), and the dropping temperature must not More than 70°C, because acrylonitrile is prone to self-polymerization when the temperature exceeds 70°C;
[0017] d. After the dropwise addition, at a temperature of 25-70°C, preferably at a temperature of 30-65°C, keep the reaction going on for 2.5-24 hours, and detect that the convers...
Embodiment 1
[0026] Add 12.002 grams (0.2 mol) of ethylenediamine (hereinafter referred to as EDA) and 30.000 grams of propylene glycol monomethyl ether (PM) into a 250 mL three-necked flask equipped with a condenser tube and a mechanical stirrer. At room temperature, 21.827 g (0.411 mol) of acrylonitrile (hereinafter referred to as ACN) was added dropwise, and the dropwise addition process was less than 2 hours, and the temperature was controlled below 70°C. After ACN has been added dropwise, continue to react for 24 hours at 25°C, and detect that the EDA conversion rate reaches 100% with gas chromatography (hereinafter referred to as GC). After the reaction finishes, analyze the composition of the reaction product, and the results are as shown in Table 1. The yield of N,N'-bis(2-cyanoethyl)-1,2-ethylenediamine (hereinafter referred to as BCNEDA) was 98.98%.
Embodiment 2
[0028] Add 12.002 g (0.2 mol) of EDA and 30.000 g of PM into a 250 mL three-necked flask equipped with a condenser and a mechanical stirrer. At 60°C, 21.827 g (0.411 mol) of ACN was added dropwise, and the dropwise addition process was less than 2 hours, and the temperature was controlled below 70°C. After the ACN was added dropwise, the reaction was continued for 2.5 hours at 65°C, and the conversion rate of EDA was detected to reach 100% by GC. After the reaction, the composition of the reaction product was analyzed. The results were shown in Table 1. 98.46%.
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