Method and catalyst for synthesizing 2-morpholinoethanol
A technology of morpholine ethanol and solid acid catalysts, applied in the direction of catalyst activation/preparation, physical/chemical process catalysts, chemical instruments and methods, etc., can solve the problems of high production cost, unfriendly environment, consumption of sulfuric acid, etc., and achieve production cost Low, considerable yield, less pollution effect
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Embodiment 1
[0039] Embodiment 1, a kind of fixed bed reactor, such as figure 1 As shown, it includes a nitrogen cylinder 1, a sampling pump 5 and a fixed bed reactor A, and the fixed bed reactor A includes a vaporization chamber 11 and a catalyst bed 6 arranged in sequence from top to bottom, and the middle part of the catalyst bed 6 A catalyst is arranged, and an inert filler 7 is respectively arranged at the upper and lower ends of the catalyst. The outer surface of the catalyst bed 6 is placed in a molten salt bath 8 which is responsible for regulating the reaction temperature in the catalyst bed 6 .
[0040] After the outlet of the nitrogen cylinder 1 and the outlet of the sampling pump 5 merge, they are connected together with the top of the vaporization chamber 11; A valve 4 is set between the outlet of 5 and the confluence point; the bottom outlet of the catalyst bed 6 is connected to the condenser 9 and the valve 10 in sequence.
Embodiment 2
[0041] Embodiment 2, a kind of preparation method of solid acid catalyst, carries out following steps successively:
[0042] 1), Roasting: Spherical γ-Al 2 o 3 Baking at 800°C for 6-10h.
[0043] 2), dipping:
[0044] Get the spherical gamma-Al after the roasting of step 1) gained 2 o 3 1000g is immersed in the ferric nitrate solution of 1000g, the mass concentration of ferric nitrate solution is 20%; Then add cobalt nitrate solution by the molar ratio of Fe:Co=2:1, the mass concentration of cobalt nitrate solution is 12%; Add as dispersant 500mL of ethanol was used to form a reaction system, and the pH value of the above reaction system was adjusted to 8.0 with ammonia water at a speed of 1000-1500rpm, so that the solid precipitation was complete.
[0045] 3), aging:
[0046] The above-mentioned reaction system after adjusting the pH value was aged at room temperature for 24 hours and then filtered. The obtained precipitate was washed with water until neutral and then ...
Embodiment 3
[0052] Embodiment 3: A kind of method of synthesizing 2-morpholine ethanol
[0053] 1), get the solid acid catalyst 300ml that embodiment 2 synthesizes and put in the catalyst bed layer 6 of the fixed-bed reactor that embodiment 1 gains.
[0054] 2) 100 g of the raw material triethanolamine is poured into the vaporization chamber 11 through the sampling pump 5. The temperature of the vaporization chamber 11 is 400° C., and the flow rate of the sampling pump 5 is adjusted so that the volumetric space velocity is 0.25 h -1 . The nitrogen gas was adjusted through the pressure reducing valve 2 so that the reaction pressure was 1.2 atm and the reaction temperature was 280°C. The product flowed out from the bottom of the fixed bed reactor A and was collected after being condensed by the condenser 9 to obtain 95 g of the reaction liquid. The lost components are carried away by nitrogen and adsorbed on the catalyst without desorption. The reaction solution was rectified under reduce...
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