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Two Preparation Tris Hydroxymethyl Aminomethane,
121.14g Tris Hydroxymethyl Aminomethane,
Two Preparation TRIS Base
Which of the two preparation methods of tris(hydroxymethyl)aminomethane is better,TRIS base manufacturer
Tris(hydroxymethyl)aminomethane is an important biochemical, chemical and pharmaceutical intermediate. Its preparation generally takes nitromethane and formaldehyde as raw materials, and obtains solid tris (hydroxymethyl) nitromethane after condensation, cooling and crystallization, and then reduces to produce tris (hydroxymethyl) aminomethane. Desheng compared the direct method and the two-step method to synthesize tris(hydroxymethyl)aminomethane, studied the catalyst regeneration, and obtained reliable technical data, which has obvious social and economic benefits.
The condensation reaction device adopts a 500L enamel reactor, a frame stirrer, and a stainless steel baffle inside. The stirring speed is 68 Y/min. The catalytic hydrogenation unit uses a 680L autoclave, double-deck paddle stirrer, and the stirring speed is 120 Y/min. The hydrogenation unit is equipped with a hydrogen pressure regulator, a stirring speed regulator, a reaction temperature controller, and cooling water.
Two methods to produce tris base
|1||Direct hydrogenation method to produce TRIS|
|2||Two-step production of TRIS|
Direct hydrogenation method to produce TRIS
Put the condensation reaction solution into a 2.0L autoclave, add 650 mol methanol, 10 ml dichloromethane, and 12 g Raney nickel. After the autoclave has passed the leak test, use nitrogen and hydrogen to switch 4 to 5 times, start the stirrer, and adjust the speed. Slowly increase the temperature, then add hydrogen, the reaction temperature rises to the specified temperature, and react for 2.5 hours at the specified temperature and pressure. After the reaction is completed, the filtrate is poured into a beaker, cooled to -5 ℃ with brine, and the white crystals are separated out. After filtration, the filtrate was concentrated under reduced pressure, and then cooled to crystallize by suction filtration, treated in the same way for 3 times, and the product was dried in vacuum.
Two-step production of TRIS
Weigh 120 g of tris (hydroxymethyl) nitromethane (THNM), 500 g of methanol, 15 g of dichloromethane, and 12 g of Raney nickel (wet product) and add them to the autoclave in turn. After the autoclave passed the leak test, replace it with nitrogen and hydrogen 4 to 5 times, start the stirrer, and adjust the speed. Slowly increase the temperature, and then add hydrogen. The reaction temperature is increased to 50-55 ℃, the pressure is 2.0-2.5 MPa, and the reaction is at this temperature for 2.5 hours. After the reaction, the catalyst is filtered off, the reaction liquid is cooled and crystallized, and the product is vacuum dried.
Comparison of the two methods
1. Compared with the two-step method to produce tris(hydroxymethyl)aminomethane, the direct method is stable, but the yield is lower. The yield is mainly determined by the yield of the condensation reaction. In the condensation reaction, except for the Conicaro reaction In addition, there are other side reactions, and it is clear that these side reactions are also the key to improving the yield.
2. The cost of paraformaldehyde, one of the raw materials of the direct hydrogenation method, is high, and the crude product refining is more cumbersome than the two-step method. Therefore, the cost of the tris(hydroxymethyl)aminomethane produced by the direct hydrogenation method is higher than that of the tris(hydroxymethyl)aminomethane produced by the two-step method. The cost of methyl)aminomethane, it is recommended to use two-step method to produce tris(hydroxymethyl)aminomethane.
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