반응 #445337

반응 방정식

sodium hydrogenphosphate

ammonia water

lanthanum nitrate

ammonia water

α-hydroxyisobutyramide

methanol

→

methacrylic acid

methyl methacrylate

용매

water

water

반응 조건

후처리

1. 1
   workup.ADDITIONwas added
2. 2
   기타a white precipitate was formed
3. 3
   세척washed by the decantation method
4. 4
   기타followed by separation by filtration and water-
5. 5
   세척washing
6. 6
   기타The resulting white precipitate was dried at 120° C.
7. 7
   workup.WAITcalcined at 400° C. for 6 hours in a stream of air
8. 8
   기타The LaPO4 catalyst (5 cc) thus obtained
9. 9
   기타was packed in a Pyrex reaction tube of 12-mm inside diameter, which
10. 10
    기타held at 275° C
11. 11
    workup.WAITwas passed through the catalyst layer at a liquid hourly space velocity of 0.5 liter/liter/hr for 30 minutes
12. 12
    기타The gas leaving the catalyst layer
13. 13
    기타was trapped in a dry ice trap

실험 절차

Next, when 100 cc of an aqueous solution containing 20.3 g (0.143 mole) of sodium hydrogenphosphate (Na2HPO4) was added, a white precipitate was formed. After stirring this at 80° C. for one hour, the white precipitate was thoroughly water-washed by the decantation method followed by separation by filtration and water-washing. The resulting white precipitate was dried at 120° C., calcined at 400° C. for 6 hours in a stream of air, and thereafter molded into granules of 10-16-mesh size. The LaPO4 catalyst (5 cc) thus obtained was packed in a Pyrex reaction tube of 12-mm inside diameter, which then was secured in an electric furnace held at 275° C. Next, while passing nitrogen from the top of the reaction tube through the catalyst layer at a gas space velocity of 480 liter/liter/hr, 14% ammonia water was passed through the catalyst layer at a liquid hourly space velocity of 0.5 liter/liter/hr for 30 minutes. The feed of the ammonia water was then stopped, and a feed liquid consisting of α-hydroxyisobutyramide, methanol and water in a mole ratio of 1:14:11.5 was fed at a liquid hourly space velocity of 0.26 liter/liter/hr. The gas leaving the catalyst layer was trapped in a dry ice trap coupled to the bottom of the reaction tube. When the products were quantitatively analyzed by gas chromatography, the molar yields of methyl methacrylate and methacrylic acid were 83.2% and 3.0%, respectively, based on the starting α-hydroxyisobutyramide.

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