Flow-type laboratory hydrogenation apparatus and laboratory hydrogenation process using the apparatus
A laboratory scale continuous flow hydrogenation apparatus ( 100 ) includes a reservoir ( 104 ), a feed pump ( 102 ), a mixing element ( 108 ) with two inlets and an outlet, a hydrogenation reactor ( 110 ) and a pressure-adjusting unit ( 112 ), all connected into a flow path. A hydrogen source ( 126 ) and a one-way valve ( 120 ) are arranged between the hydrogen source ( 126 ) and the second inlet of the mixing element ( 108 ). The feed pump ( 102 ) can provide a constant volume rate. The reservoir ( 104 ) contains at least a solvent base solution of the sample to be hydrogenated. The hydrogenation reactor ( 110 ) connects into the flow path by detachable connections and is formed as a replaceable cartridge containing a packing which increases the flow resistance and facilitates mixing. The pressure-adjusting unit ( 112 ) connects into the flow path after the hydrogenation reactor ( 110 ) and is provided with a regulation controlled electrically.
1. A laboratory scale continuous flow hydrogenation apparatus ( 100 ; 200 , 300 ) for hydrogenating given samples below supercritical pressure values, comprising:
a reservoir ( 104 ; 204 ),
a feed pump ( 102 ; 202 ),
a collecting element ( 108 ; 208 ) with two inlets and an outlet,
a hydrogenation reactor ( 110 ; 210 , 310 - 1 , . . . , 310 -m), and a pressure-adjusting unit ( 112 ; 212 ), all connected into a flow path,
a hydrogen source ( 126 ; 226 ), and
a valve ( 120 ; 220 ) configured to transmit a gas stream only into a single direction and connected between the hydrogen source ( 126 ; 226 ) and the second inlet of the collecting element ( 108 ; 208 ), wherein the pressure-adjusting unit ( 112 ; 212 ) is connected into the flow path after the hydrogenation reactor ( 110 ; 210 , 310 - 1 , . . . , 310 -m),
wherein said feed pump ( 102 ; 202 ) is a pump with a constant volume rate and the reservoir ( 104 ; 204 ) contains at least a solvent, as a base solution, of the sample to be hydrogenated, and wherein the hydrogenation reactor ( 110 ; 210 , 310 - 1 , . . . , 310 -m) is joined into the flow path via detachable connections and is formed as a replaceable cartridge with a packing in its inner space configured to increase the flow resistance and facilitate the mixing of liquid and gaseous components, and wherein the pressure-adjusting unit ( 112 ; 212 ) is provided with an electrically controlled regulator having a control range of a ratio of at least 1:6, the regulator being configured to maintain a given pressure in the flow path and for tuning said pressure in quasi-continuous steps, with the base solution flowing through the reactor ( 110 ; 210 , 310 - 1 , . . . , 310 -m) to a value that falls below supercritical pressure values of the base solution.
2. The laboratory scale hydrogenation apparatus ( 200 , 300 ) according to claim 1 , comprising at least one sample container ( 240 ) containing the liquid sample or a solution thereof, wherein the sample container ( 240 ) is separated from the reservoir ( 204 ) and is connected through a dosing injector ( 242 ) to a section of the flow path situated between the feed pump ( 202 ) and the collecting element ( 208 ), and wherein the reservoir ( 204 ) contains only the solvent of the sample to be hydrogenated.
3. The laboratory scale hydrogenation apparatus ( 100 ; 200 , 300 ) according to claim 1 , comprising a hydrogen source ( 126 ; 226 ) generating the gaseous hydrogen in-situ.
4. The laboratory scale hydrogenation apparatus ( 100 ; 200 , 300 ) according to claim 3 , wherein the hydrogen source ( 126 ; 226 ) is formed by at least one asymmetric pressure electrolytic cell configured to generate gaseous hydrogen with a pressure being higher than said pressure maintained in the flow path.
5. The laboratory scale hydrogenation apparatus ( 100 ; 200 , 300 ) according to claim 1 , wherein the packing of the hydrogenation reactor ( 110 ; 210 , 310 - 1 , . . . , 310 -m) comprises a catalyst necessary for the hydrogenation.
6. The laboratory scale hydrogenation apparatus ( 300 ) according to claim 2 , comprising a plurality of hydrogenation reactors ( 310 - 1 , . . . , 310 -m) which are connected into the flow path through a switching valve ( 360 ) having a multiway construction at least on the inlet side thereof.
7. The laboratory scale hydrogenation apparatus ( 300 ) according to claim 2 , comprising a plurality of sample containers ( 340 - 1 , . . . , 340 -n), wherein the outlet of each sample container ( 340 - 1 , . . . , 340 -n) is connected through a switching valve ( 350 ) to the sample injector ( 242 ).
8. The laboratory scale hydrogenation apparatus ( 100 ; 200 , 300 ) according to claim 1 , comprising a central controlling electronics ( 116 ; 216 ) which is connected through appropriate electric connections with the valve ( 120 ; 220 ), the pressure-adjusting unit ( 112 ; 212 ) and the feed pump ( 102 ; 202 ).
9. The laboratory scale hydrogenation apparatus ( 100 ; 200 , 300 ) according to claim 8 , comprising a heating/cooling means ( 130 ; 230 ) inserted between the outlet of the collecting element ( 108 ; 208 ) and the inlet of the hydrogenation reactor ( 110 ; 210 , 310 - 1 , . . . , 310 -m), wherein the heating/cooling means ( 130 ; 230 ) is electrically connected with the controlling electronics ( 116 ; 216 ).
10. The laboratory scale hydrogenation apparatus ( 100 ; 200 , 300 ) according to claim 1 , wherein the total inner volume measured along the flow path from the feed pump ( 102 ; 202 ) to the pressure-adjusting unit ( 112 ; 212 ) is at most 10 cm 3 .
11. A laboratory scale continuous flow hydrogenation apparatus ( 100 ; 200 , 300 ) for hydrogenating given samples below supercritical pressure values, comprising:
a reservoir ( 104 ; 204 ),
a feed pump ( 102 ; 202 ),
a collecting element ( 108 ; 208 ) with two inlets and an outlet, and
a hydrogenation reactor ( 110 ; 210 , 310 - 1 , . . . , 310 -m), and a pressure-adjusting unit ( 112 ; 212 ), all connected into a flow path, and
a hydrogen source ( 126 ; 226 ) configured to form an integral part of said apparatus ( 100 ; 200 , 300 ) as at least one asymmetric pressure electrolytic cell and a valve ( 120 ; 220 ) configured to transmit a gas stream only into a single direction and connected between said hydrogen source ( 126 ; 226 ) and the second inlet of the collecting element ( 108 ; 208 ), and the pressure-adjusting unit ( 112 ; 212 ) is connected into the flow path after the hydrogenation reactor ( 110 ; 210 , 310 - 1 , . . . , 310 -m),
wherein said feed pump ( 102 ; 202 ) is a pump with a constant volume rate and the reservoir ( 104 ; 204 ) contains at least a solvent, as a base solution, of the sample to be hydrogenated, and wherein the hydrogenation reactor ( 110 ; 210 , 310 - 1 , . . . , 310 -m) is joined into the flow path via detachable connections and is formed as a replaceable cartridge with a packing in its inner space configured to increase the flow resistance and facilitate the mixing of liquid and gaseous components, and wherein the pressure-adjusting unit ( 112 ; 212 ) is provided with an electrically controlled regulator having a control range of a ratio of at least 1:6, the regulator being configured to maintain a given pressure in the flow path and for adjusting said pressure with the base solution flowing through the reactor ( 110 ; 210 , 310 - 1 , . . . , 310 -m) to a value that falls below supercritical pressure values of the base solution.
12. The laboratory scale hydrogenation apparatus ( 100 ; 200 , 300 ) according to claim 11 , wherein the at least one asymmetric pressure electrolytic cell is an asymmetric pressure electrolytic cell configured to generate gaseous hydrogen with a pressure ranging from 1 to 500 bar.