Preparing method of tetramethylethylenediamine
A technology of tetramethylethylenediamine and ethylenediamine, applied in the field of preparation of tetramethylethylenediamine, can solve the problems of inability to achieve clean production, large amount of aqueous formaldehyde solution, large number of methylation, etc. Low, high purity, high yield effect
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[0021] The invention provides a kind of preparation method of tetramethylethylenediamine, comprises the following steps:
[0022] Paraformaldehyde is dissolved in an organic solvent to obtain a paraformaldehyde solution;
[0023] In the presence of a catalyst and hydrogen, the paraformaldehyde solution and ethylenediamine are subjected to a methylation hydrogenation reaction, and the obtained reaction liquid is rectified to obtain tetramethylethylenediamine.
[0024] The present invention uses paraformaldehyde as a raw material, dissolves the paraformaldehyde with an organic solvent, avoids the use of formaldehyde aqueous solution, or avoids the difficult-to-handle salt wastewater containing sodium chloride produced after using dichloroethane as a raw material; the process is simple and easy Operation, low cost, and higher yield of tetramethylethylenediamine.
[0025] The invention dissolves paraformaldehyde in an organic solvent to obtain a paraformaldehyde solution. In the...
Embodiment 1
[0043]Weigh 200g of methanol, raise the temperature to 45°C, add 130g of paraformaldehyde, heat the organic solvent to 45°C for 1 hour, stir and dissolve, then cool down to 20°C to 25°C to obtain a mixed solution, which is used as a reaction raw material for four Synthesis reaction of methylethylenediamine. Add 60g of ethylenediamine, 0.3g of 5% palladium carbon catalyst, nitrogen and hydrogen to the autoclave for replacement, heat up to 120°C and pass through hydrogen, pressure to 2.8-3.2Mpa, pump the mixed solution into the autoclave at a rate of 70g / h, methylation and hydrogenation reaction, after the reaction, the reaction liquid was rectified to obtain 114g of tetramethylethylenediamine, the product content was 99.64%. Measure the water content and conversion rate of raw materials in the system. The test data are shown in Table 1.
[0044] The present invention carries out proton nuclear magnetic resonance spectrum test to the tetramethylethylenediamine prepared by embo...
Embodiment 2
[0046] Weigh 260g of tetramethylethylenediamine, raise the temperature to 55°C, add 130g of paraformaldehyde, heat the organic solvent to 60°C for 1 hour, stir and dissolve, then cool down to 20°C to 25°C to obtain a mixed solution, as The reaction raw materials are used for the synthetic reaction of tetramethylethylenediamine. Add 60g of ethylenediamine, 0.3g of 5% palladium-carbon catalyst, nitrogen and hydrogen to the autoclave for replacement, heat up to 120°C and pass through hydrogen, and pump the mixed solution into the autoclave at a rate of 70g when the pressure reaches 2.8-3.2MPa / h, methylation and hydrogenation reaction, after the reaction, the reaction solution was rectified, and 371.8 g of tetramethylethylenediamine was obtained by separation, with a product content of 99.43. Measure the water content and conversion rate of raw materials in the system. The test data are shown in Table 1.
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