The preparation method of polyol amine
A polyolamine and alcoholamine technology, which is applied in the preparation of organic compounds, chemical instruments and methods, preparation of aminohydroxy compounds, etc., can solve the problems of long post-treatment process, environmental pollution by waste water, and high reaction pressure, and achieve product yield. High, high conversion rate of raw materials, mild reaction conditions
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[0028] A kind of preparation method of polyol amine, comprises process as follows:
[0029] Mix dichloropropane and alcohol amine in a molar ratio of 1:1 to 4, dichloropropane and alkali catalyst in an equivalent ratio of 1:1 to 4, mix to form a uniform slurry, and feed it into the tubular screw propulsion reactor from the feeding port. The set reaction temperature of the tubular screw propulsion reactor is 50-100°C; the propulsion line speed is 0.10-1.00m / min, and the rotation speed is 10.00-100.00rad / min. At the set temperature, one or two chlorines of dichloropropane are replaced by amino alcohols to generate monosubstituted polyol amine or disubstituted polyol amine products, and at the same time generate by-product industrial salts.
[0030] Driven by the screw propulsion reactor, the industrial salt precipitated during the reaction is propelled from the tubular reactor to the salt collector to discharge the reaction system. The reaction system after desalination is filt...
Embodiment 1
[0033] Coconut shell charcoal was roasted at 300°C in a nitrogen atmosphere for 6h, cooled and soaked in 7mol / L sodium hydroxide aqueous solution for 6h, filtered and washed with distilled water for 4 times, dried at 120°C for 6h, then soaked in 7mol / L nitric acid aqueous solution for 8h, The coconut shell charcoal was washed with distilled water for 3 times, dried at 120°C for 6 hours after filtration, and roasted at 300°C for 6 hours for later use.
[0034] The processed granular coconut shell charcoal, sodium hydroxide and lanthanum nitrate are mixed according to the mass ratio of 100:5:1, and sodium hydroxide and lanthanum nitrate are prepared into a mixed solution. The coconut shell charcoal is excessively impregnated and adsorbed for 10 hours under stirring, and dried at 120°C for 8 hours. Then put it in a horse boiling furnace and roast at 350°C for 8 hours in a nitrogen atmosphere, so that sodium hydroxide and lanthanum nitrate melt and penetrate into the gap between th...
Embodiment 2
[0036]Dichloropropane, diisopropanolamine and sodium hydroxide (48.0wt%) in a molar ratio of 1:2:2 were metered and mixed to form a homogeneous solution, and then added to a tubular screw propulsion reactor. The tubular screw propulsion reactor was set at a reaction temperature of 80°C and a linear propulsion speed of 0.50m / min. The salt generated by the reaction enters the salt collector and exits the reactor under the action of the screw propeller. The reaction system after desalination was filtered and collected into the tank reactor, and the reaction was carried out at a temperature of 140° C., a stirring speed of 80.0 rad / min, and a pressure of 2.0 MPa until the pressure was stable and ended. Stripping at a temperature of 80°C and a vacuum of 0.40MPa; vacuum extraction to remove unreacted light components and water recycling to the raw material end for use, the product is filtered and desalted before being sent for inspection ( image 3 ) packaging, the conversion rate o...
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