DEVICE AND METHOD FOR CATALYTICALLY CONVERTING CHEMICAL SUBSTANCES AT DWELL TIMES IN THE RANGE OF 0.1-10 SECONDS

Abstract

Disclosed herein is an apparatus and a method for catalytic conversion of chemical substances in the presence of pulverulent catalysts in a trickle bed reactor with residence times in the range of 0.1-10 seconds, wherein the apparatus includes a trickle bed reactor (2), the inlet side of which is functionally connected to a catalyst reservoir vessel (1) and a reactant feed, and the outlet side of which is functionally connected to a separator (3). The separator (3) has an exit conduit for leading off product stream, wherein the apparatus has the characteristic feature that the exit conduit disposed on the separator (3) for leading off product stream has a continuously acting valve connected via a controller to a pressure measurement sensor, wherein the continuously acting valve and the pressure measurement sensor form a pressure control circuit with a controller.

Claims

1: An apparatus for catalytic conversion of chemical substances in the presence of pulverulent catalysts in a trickle bed reactor with residence times in the range of 0.1-10 seconds, wherein: the apparatus comprises at least a trickle bed reactor, a catalyst reservoir vessel and a separator; the reactor is a tubular reactor having a length in the range of 0.3-3 m and a diameter in the range of 0.3-10 cm; an inlet side of the reactor is functionally connected to at least one catalyst reservoir vessel and at least one reactant feed, and an outlet side of the reactor is functionally connected to the at least one separator; the at least one separator having at least one exit conduit for leading off product stream; and the apparatus has the characteristic feature that an exit conduit disposed on the separator for leading off product stream has a continuously acting valve connected via a controller to a pressure measurement sensor, in which the continuously acting valve and the pressure measurement sensor form a pressure control circuit with a controller.

2: The apparatus according to claim 1, wherein: the catalyst reservoir vessel and the separator have a functional connection equipped with a pressure differential controller that actuates a continuously acting valve; the outlet side of the valve has either a connecting conduit to the separator or a waste air conduit; and in case that the outlet side of the valve has a waste air conduit, the separator is equipped with a gas feed and the part of the functional connection between the pressure differential controller and the separator is connected to the pressure measurement sensor of the pressure differential controller.

3: The apparatus according to claim 1, wherein the apparatus has temperature control of the individual apparatus elements with which at least the apparatus elements from the group of catalyst reservoir vessel, reactor and separator are independently heatable.

4: The apparatus according to claim 1, wherein the continuously acting valve has a functional connection to a pressure measurement sensor that leads to the input region of the trickle bed reactor, to the output region of the trickle bed reactor or to the exit conduit for leading off product stream.

5: The apparatus according to claim 1, wherein: a metering unit for supply of liquid fluids selected from the group consisting of oils, heavy oils, VGO, residue oils, bio oil, biomass, pyrolysis oil, peat oil, lignin, gasoline, diesel, and naphtha, and/or the exit conduit connected to the separator for leading off product stream has a liquid separator; and the liquid separator is disposed upstream of the continuously acting valve.

6: The apparatus according to claim 1, wherein the continuously acting valve in the exit conduit for leading off product stream has a control dynamic in the region of 1:100.

7: The apparatus according to claim 1, wherein the continuously acting valve in the exit conduit for leading off product stream has a control quality having a deviation in relation to the target value of <10%.

8: The apparatus according to claim 1, wherein the continuously acting valve in the exit conduit for leading off product stream and the pressure measurement sensor connected thereto form a pressure controller of analog or digital backpressure controllers.

9: The apparatus according to claim 4, wherein the metering unit has a twin-needle injector and/or the the metering unit has a high-pressure pump.

10: The apparatus according to claim 4, wherein the exit conduit for leading off product stream is connected to a gas collection vessel.

11: A method of catalytically converting chemical substances in the presence of pulverulent catalysts with residence times in the range of 0.1-10 seconds, the method comprising: (i) adjusting the temperature of at least one catalyst which is stored in at least one catalyst reservoir vessel, (ii) supplying the catalyst in a controlled manner from the at least one catalyst reservoir vessel to the inlet of a trickle bed reactor, wherein at least the catalyst is supplied in the presence of a carrier gas, (iii) contacting the pulverulent catalyst with at least one feed and passing the mixture of catalyst, feed and carrier gas through the reaction space of the trickle bed reactor, (iv) transferring the mixture of catalyst, feed, carrier gas and products through the reactor outlet into a separator, (v) separating feed and reaction products from catalyst in the separator and removing them via an exit conduit, controlling the backpressure by a continuously acting valve during the leading-off of feed, carrier gas and products from the exit conduit connected to the separator, where the backpressure is in the range of 0.01 barg-15 barg.

12: The method of claim 11, wherein the period of time in the performance of method steps (ii)-(iii) in which pulverulent catalyst is being conveyed through the trickle reactor is a total period of time of 10-300 seconds and the changes in pressure on the outlet side of the reactor during the performance of the method are <200 mbarg.

13: The method of claim 11, wherein the sampling time of the pressure control is pulsed or continuous and the sampling time has a time in the range of 0.0001-300 seconds.

14: A method of catalytically converting chemical substances in the presence of pulverulent catalysts with residence times in the range of 0.1-10 seconds, in the apparatus of claim 1, the method comprising: adjusting the temperature of at least one catalyst which is stored in the at least one catalyst reservoir vessel, (ii) supplying the catalyst in a controlled manner from the at least one catalyst reservoir vessel to the inlet of the trickle bed reactor, wherein at least the catalyst is supplied in the presence of a carrier gas, (iii) contacting the pulverulent catalyst with at least one feed and passing the mixture of catalyst, feed and carrier gas through the reaction space of the trickle bed reactor, (iv) transferring the mixture of catalyst, feed, carrier gas and products through the reactor outlet into the separator, (v) separating feed and reaction products from catalyst in the separator and removing them via the exit conduit, controlling the backpressure by the continuously acting valve during the leading-off of feed, carrier gas and products from the exit conduit connected to the separator, where the backpressure is in the range of 0.01 barg-15 barg.

Description

BRIEF DESCRIPTION OF THE FIGURES

[0083] FIG. 1 shows the schematic diagram of an apparatus having a trickle bed reactor (2), specifically having an arrangement on the reaction space exit side of separator (3) functionally connected via the exit conduit to liquid separator (9) and gas collection vessel (4). The actuator valve (12) is disposed in the exit conduit between the separator (3) and the liquid separator (9), and the pressure control valve (7) between the liquid separator (9) and the gas collection vessel (4).

[0084] FIG. 2.a shows the schematic diagram of an apparatus in one configuration of the invention with a trickle bed reactor (2), in this embodiment with a pressure regulator (7) disposed in the exit conduit leading from the liquid separator (9) to the gas collection vessel (4) that can take its actual value from different points in the apparatus. The actual pressure value may be in the region of the inlet to the trickle bed reactor (2), in the region of the outlet from the trickle bed reactor (2) or in the region of the gas exit conduit. The functional connection (21) leads to the inlet of the trickle bed reactor (2); the functional connection (20) leads to the inlet of the separator (3) and is close to the exit from the trickle bed reactor (2). The functional connection (22) shows the embodiment with taking of the actual pressure value close to the continuously acting valve of the pressure controller (7).

[0085] FIG. 2.b shows a schematic diagram of the embodiment of the pressure controller (7) as a secondary stream pressure control system.

[0086] FIG. 2.c shows a schematic diagram of the embodiment of a pressure controller (7) by means of a relief valve. This is a specific embodiment with a membrane relief valve having the characteristic feature that the actual pressure value is taken in the valve itself.

[0087] FIG. 2.d shows a schematic diagram of the apparatus of the invention equipped with a separate gas supply (18). The separator (3) is functionally connected to the negative target value input of the pressure differential controller (6), while the positive target value input of the pressure differential controller (6) is functionally connected to the catalyst reservoir vessel (1). There is a further functional connection between the reservoir vessel (1) and the input of a valve which is actuated by the pressure controller (6). The output from the valve is configured as a waste air conduit (19). An auxiliary gas is likewise supplied via conduit (17), which, especially with the valve (10) closed, ensures that catalyst powder above the valve is loosened and hence remains free-flowing.

[0088] FIG. 3 shows pressure progressions in the performance of the catalytic analysis by the method of the invention (see experimental example EB1 with dotted line) and by the method corresponding to the prior art (see comparative example VB1 with solid line). The initial pressure at the start of each analysis was identified by PA in the figure. The duration of each cracking experiment is about 60 seconds, with the commencement identified by start and the end by stop.

[0089] FIG. 4 shows formation of propene as a function of the conversion established by the ratio of catalyst to oil (i.e. the C/O ratio or the cat/oil ratio). The figure for the propene yield and the conversion are reported in % by weight. The measurement series S1, S2 and S3 show the data that have been achieved at the pressures of 0.5 bar, 1.5 bar and 2.5 bar by the method of the invention. The measurement series VS1 and VS2 show the data that have been performed by the comparative experiments, with the starting pressures (in the case of VS2) at 0.5 bar and (in the case of VS1) at 1.2 bar.

LIST OF REFERENCE SIGNS

[0090] 1Catalyst reservoir vessel [0091] 2Trickle bed reactor [0092] 3Separator with an inner region divided by a porous plate for storage of the catalyst in the fluidized state [0093] 4Gas collection vessel [0094] 5Pressure measurement sensor in the catalyst reservoir vessel or in the gas supply conduit to the catalyst reservoir vessel [0095] 6Pressure differential controller functionally connected between catalyst reservoir vessel (1) and trickle bed reactor (2) [0096] 7Pressure regulator in the exit conduit, functionally connected to the separator (3) [0097] 8Liquid reservoir vessel [0098] 9Liquid separator [0099] 10Valve to release the catalyst flow [0100] 12Valve in the exit conduit between the separator (3) and the liquid separator (9) [0101] 14Pump, preferably a high-pressure pump [0102] 15Pressure measurement sensor connected to the liquid supply or the reactor inlet [0103] 16Pressure measurement sensor connected to the conduit between pressure differential controller (6) and separator (3) [0104] 17Gas conduit supply [0105] 18Gas supply [0106] 19Waste air conduit [0107] 20Actual pressure value in the gas supply to the separator (3) and hence functionally connected to the trickle bed reactor (2) [0108] 21Actual pressure value at the reactor inlet [0109] 22Actual pressure value in the conduit downstream of the liquid separator (9), which is thus likewise characteristic of the pressure in the region of the reactor exit