CN101905139A - Device and method for evaluating catalyst - Google Patents
Device and method for evaluating catalyst Download PDFInfo
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- CN101905139A CN101905139A CN 201010228855 CN201010228855A CN101905139A CN 101905139 A CN101905139 A CN 101905139A CN 201010228855 CN201010228855 CN 201010228855 CN 201010228855 A CN201010228855 A CN 201010228855A CN 101905139 A CN101905139 A CN 101905139A
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Abstract
The invention provides a device and a method for evaluating a catalyst. The device for evaluating the catalyst comprises an air inlet pipeline, a raw material pipeline, a fixed bed micro-reactor, a fixed bed heating furnace, a fluidized bed reactor and a fluidized bed heating furnace, wherein the fixed bed micro-reactor is connected with the air inlet pipeline and the raw material pipeline; the fixed bed heating furnace accommodates the fixed bed micro-reactor; the fluidized bed reactor is connected with the air inlet pipeline, the raw material pipeline and the fixed bed heating furnace; and the fluidized bed heating furnace accommodates the fluidized bed reactor. The invention also discloses a method for evaluating the catalyst. In the method, the fixed bed micro-reactor adopts a manual or automatic feeding mode. The device and the method solve the problems of high investment, complex operation and the like of a catalyst evaluation system due to separate design of the conventional fixed bed micro-reactor and fluidized bed reactor.
Description
Technical field
The present invention relates to a kind of apparatus and method that are used for evaluating catalyst.
Background technology
The evaluating catalyst system is the device that catalyst activity, selectivity etc. is estimated, and fixed-bed micro-reactor is laboratory catalyst development, the evaluating apparatus of using always.The fluid bed microreactor is usually used under fluidized state estimating catalytic performances such as the activity, selectivity of preformed catalyst.
In the prior art, general fixed-bed micro-reactor and fluid bed microreactor adopt two cover independent device usually.Every cover evaluating apparatus all need be furnished with core parts such as gas handling system, gas flow control system, reaction system, heating and temperature-controlling system, analyzing and testing system.Fixed-bed micro-reactor and fluid bed microreactor design separately separately and make that the investment of evaluating catalyst system is high, complicated operation.
Summary of the invention
The present invention aims to provide a kind of device that integrates catalyst fixed bed microreactor evaluation and fluid bed microreactor Function of Evaluation, with solve fixed-bed micro-reactor and fluid bed microreactor separately separately design make that the investment of evaluating catalyst system is high, problems such as complicated operation.By the switching of a plurality of valves, realize the switching of fixed-bed micro-reactor pulse sample introduction and continuous sample introduction mode.Solved one and overlapped the evaluation that fixed-bed micro-reactor can be applied to liquid charging and gas feed reaction system catalyst.Fixed fluidized bed microreactor is realized the performance evaluation of catalyst under the fluidized state, and is simple to operate.The present invention have operate steadily, the outstanding advantage of rational in infrastructure, diverse in function, help improving catalyst development efficient.
According to an aspect of the present invention, provide a kind of device that is used for evaluating catalyst, having comprised: the assist gas pipeline; The unstrpped gas pipeline; Fixed-bed micro-reactor is connected with the unstrpped gas pipeline with the assist gas pipeline; The fixed bed heating furnace, the heating fixed-bed micro-reactor; The fluid bed microreactor is connected with assist gas pipeline, unstrpped gas pipeline, fixed-bed micro-reactor export pipeline; Fluidized bed furnace, the heated fluidized bed microreactor.
Further, be used for the device of evaluating catalyst, also comprise: valve control system; Fixed-bed micro-reactor is connected with the unstrpped gas pipeline with the assist gas pipeline by valve control system; The fluid bed microreactor is connected with assist gas pipeline, unstrpped gas pipeline, fixed-bed micro-reactor export pipeline by valve control system.
Further, valve control system comprises: first six-way valve, second six-way valve, the 3rd six-way valve, the 4th triple valve, the 5th triple valve; The device of evaluating catalyst also comprises: first quantity tube;
First six-way valve, its first end connects the carrier gas interface of chromatogram, and its 3rd end connects assist gas pipeline and unstrpped gas pipeline, and its 4th end is connected with first end of the 4th triple valve, and its 6th end is connected with first end of second six-way valve; Second end, five terminal are connected with first quantity tube respectively;
Second end of the 4th triple valve is the first emptying end, and the 3rd end of the 4th triple valve connects the 3rd end of second six-way valve;
Second end of second six-way valve is connected and fixed the inlet of a microreactor, and its five terminal connects the fluid bed microreactor and the fixed-bed micro-reactor port of export;
The 3rd six-way valve, its first end connects the carrier gas interface of gas-chromatography, its second end connects the 6th end of second six-way valve, switch according to the experiment needs with the 3rd end of the 3rd six-way valve, the quantity tube that the 6th end links to each other, its the 4th end is by connecting the 4th end of second six-way valve, and its five terminal is the second emptying end.
Further, valve control system also comprises: the 5th triple valve, the 4th end of the 3rd six-way valve connects the 4th end of second six-way valve by first end of the 5th triple valve, connect the 4th end of second six-way valve by second end of the 5th triple valve, the 3rd end of the 5th triple valve is off-line gas or calibrating gas injection port.
Further, first six-way valve is pneumatic control formula six-way valve or electronic control formula six-way valve.
Further, the 3rd six-way valve is pneumatic control formula six-way valve or electronic control formula six-way valve.
Further, be used for the device of evaluating catalyst, also comprise: the 3rd triple valve, its first end connects assist gas pipeline and unstrpped gas pipeline, its second end connects second end of first six-way valve, and its 3rd end connects the arrival end at the top of fluid bed microreactor.
Further, the assist gas road comprises: air pipe line, nitrogen pipeline and second triple valve, and first end of second triple valve connects air pipe line, and its second end connects nitrogen pipeline, and its 3rd end is connected with first end of the 3rd triple valve.
Further, the unstrpped gas pipeline comprises: the first unstrpped gas pipeline, the second unstrpped gas pipeline and first triple valve, first end of first triple valve connects the first unstrpped gas pipeline, and its second end connects the second unstrpped gas pipeline, and its 3rd end is connected with first end of the 3rd triple valve.
Further, the unstrpped gas pipeline also comprises: flow control system.
Further, flow control system is connected between first end of the 3rd end of first triple valve and the 3rd triple valve.
Further, flow control system comprises: the pressure-reducing valve of series connection, magnetic valve, check valve and mass flowmenter wherein, are provided with check valve before the mass flowmenter.
Further, fixed-bed micro-reactor comprises: fixed-bed micro-reactor main body, gas vent, be arranged on the liquid-inlet and the gas access on described fixed-bed micro-reactor main body top.
The present invention has also improved a kind of method that is used for evaluating catalyst, wherein, uses the foregoing device that is used for evaluating catalyst, and fixed-bed micro-reactor adopts manual charging or adopts automatic feed.
Further, fluid bed microreactor automatic feed.
Because fixed-bed micro-reactor is connected with the unstrpped gas pipeline with the assist gas pipeline; And the fluid bed microreactor is connected with assist gas pipeline, unstrpped gas pipeline, fixed-bed micro-reactor outlet line; Fixed-bed micro-reactor and the shared identical gas-chromatography of fluid bed microreactor outlet product gas.So, the device that is used for evaluating catalyst of the present invention fixed-bed micro-reactor estimate and the fluid bed microreactor in can shared one overlap assist gas pipeline, unstrpped gas pipeline, mass flowmenter and product gas quantitative analysis device, so overcome existing fixed bed microreactor and fluid bed microreactor separately separately design make evaluating catalyst system investment high, problems such as complicated operation.
Description of drawings
Constitute this specification a part, be used for further understanding accompanying drawing of the present invention and schematically shown the preferred embodiments of the present invention, and be used for illustrating principle of the present invention with specification.Among the figure:
Fig. 1 has schematically shown structure and the operation principle according to the device that is used for evaluating catalyst of the embodiment of the invention;
Fig. 2 has schematically shown the structure according to the fixed-bed micro-reactor of the embodiment of the invention.
The specific embodiment
Need to prove that under the situation of not conflicting, embodiment and the feature among the embodiment among the application can make up mutually.Describe the present invention below with reference to the accompanying drawings and in conjunction with the embodiments in detail.
As shown in Figure 1, the device that is used for evaluating catalyst according to the embodiment of the invention comprises: the assist gas pipeline; The unstrpped gas pipeline; Fixed-bed micro-reactor R1 is connected with the unstrpped gas pipeline with the assist gas pipeline; Fixed bed heating furnace HT1, heating fixed-bed micro-reactor R1; Fluid bed microreactor R2 is connected with additional-air inlet pipeline, unstrpped gas pipeline, fixed-bed micro-reactor export pipeline; Fluidized bed furnace HT2, heated fluidized bed microreactor R2.Fixed bed heating furnace HT1 and fluidized bed furnace HT2 can carry out the temperature control heating by temperature-control heat couple is set, and to obtain suitable reaction temperature, measure the temperature of reactor diverse location by temperature thermocouple is set.
Assist gas pipeline and unstrpped gas pipeline are used to provide required complementary gas of evaluating catalyst and different material gas.The assist gas pipeline comprises the N from the chromatographic analysis system 30 (abbreviation chromatogram) and the spectrum of discoloring
2Carrier gas system and other air inlet pipelines.Different phase and reaction needed according to evaluating catalyst, the gas that air inlet pipeline comprises and is used for beds activation, purges, be used to dilute unstrpped gas, post catalyst reaction bed during reaction is carried, the gas piping of catalyst regeneration, and for example air inlet pipeline comprises: air pipe line 15, nitrogen pipeline 17.According to different reactions, the composition of supplying raw materials in the unstrpped gas pipeline can be different, for example the unstrpped gas pipeline comprises: the first unstrpped gas pipeline 11, the dimethyl ether pipeline during dimethyl ether system olefine reaction for example, the second unstrpped gas pipeline 13 for example can provide the C when comprising the higher hydrocarbons cracking reaction
4, C
5Or C
6Gas, 2-butylene gas during isomerization reaction, ethene during disproportionated reaction and butylene.The composition of the reacting gas in the unstrpped gas pipeline of the present invention is not limited to said components, can select as required.
Because fixed-bed micro-reactor is connected with the unstrpped gas pipeline with the assist gas pipeline; And the fluid bed microreactor is connected with assist gas pipeline, unstrpped gas pipeline, fixed-bed micro-reactor outlet line; Fixed-bed micro-reactor and the shared identical gas-chromatography of fluid bed microreactor outlet product gas.So, the device that is used for evaluating catalyst of the present invention fixed-bed micro-reactor estimate and the fluid bed microreactor in can shared one overlap assist gas pipeline, unstrpped gas pipeline and product gas quantitative analysis device, so overcome existing fixed bed microreactor and fluid bed microreactor separately separately design make evaluating catalyst system investment high, problems such as complicated operation.
Further, the device that is used for evaluating catalyst also comprises: valve control system; Fixed-bed micro-reactor R1 is connected with the unstrpped gas pipeline with the assist gas pipeline by valve control system; Fluid bed microreactor R2 is connected with assist gas pipeline, unstrpped gas pipeline, fixed bed minisize reaction export pipeline by valve control system.This valve control system can be made of a plurality of valves, with realization each stage of valve control system is controlled air feed and supplies raw material.Can realize the switching of fixed-bed micro-reactor and fluid bed microreactor by the switching of valve in the valve control system, to realize the switching of fixed bed reaction and fluidized-bed reaction.The present invention has realized fixed bed reaction and these two kinds of functions of fluidized-bed reaction with a sleeving valve gate control system, having solved reaction of existing fixed bed and fluidized-bed reaction needs to be provided with separately separately, can not concentrate on a problem in the device, simplified the connection of equipment, reduce required equipment, thereby reduced the cost and the occupation of land of equipment.
Further, valve control system comprises: the first six-way valve 6V1, the second six-way valve 6V2, the 3rd six-way valve 6V3, the 4th triple valve 3V4, the 5th triple valve 3V5.The device of evaluating catalyst also comprises: first quantity tube 32.
The first six-way valve 6V1, have six ends, its first end connects the carrier gas interface from gas-chromatography, its the 3rd end connects assist gas pipeline and unstrpped gas pipeline, its the 4th end is connected with first end of the 4th triple valve 3V4, its the 6th end is connected with first end of the second six-way valve 6V2, and second end of first six-way valve, five terminal are connected with first quantity tube 32 respectively; Adopt six-way valve can realize connecting easily, according to the variation of feed state, switching is connected in the quantity tube of second end, five terminal and the connection status at other two ends of 6V1.
Second end of the 4th triple valve 3V4 is the first emptying end, and to carry out emptying, the 3rd end of the 4th triple valve 3V4 connects the 3rd end of the second six-way valve 6V2.
Second end of the second six-way valve 6V2 is connected and fixed the inlet of microreactor R1, and its five terminal is connected and fixed the outlet line of a microreactor R1 and fluid bed microreactor R2.
The 3rd six-way valve 6V3, have six ports, its first end connects the gas-carrier pipeline (abbreviation carrier gas) 35 that enters chromatographic analysis system 30 injection ports, its second end connects the 6th end of the second six-way valve 6V2, its the 4th end connects the 4th end of the second six-way valve 6V2 by 3V5, its five terminal is the second emptying end, to carry out emptying.Further, the 3rd six-way valve is the 3rd six-way valve 6V3.Its effect and the first six-way valve 6V1 are similar.
By the first six-way valve 6V1, the second six-way valve 6V2, the 3rd six-way valve, the 4th triple valve 3V4, the 5th triple valve 3V5, the device that is used for evaluating catalyst of the present invention can realize controlling easily and flexibly the switching of assist gas pipeline and unstrpped gas pipeline, control the process of evaluating catalyst exactly, can pass through this several Control valve, a shared cover air inlet pipeline, raw material pipeline, thereby do not need design separately separately as existing fixed bed microreactor and fluid bed microreactor, connect air inlet pipeline and raw material pipeline separately separately.The present invention organically is combined in fixed-bed micro-reactor and fluid bed microreactor in the device and uses, so reduced the investment of evaluating catalyst system, has saved equipment occupation space, has simplified operation.
Further, valve control system also comprises: the 5th triple valve 3V5, the 4th end of the 3rd six-way valve connects the 4th end of the second six-way valve 6V2 by first end of the 5th triple valve 3V5, connect the 4th end of the second six-way valve 6V2 by second end of the 5th triple valve 3V5, the 3rd end of the 5th triple valve 3V5 is an off-line gas sampling mouth 31.The 5th triple valve 3V5 has realized off-line gas analysis or calibrating gas sample analysis easily, and operation is simple.Further, be used for the device of evaluating catalyst, also comprise: the 3rd triple valve 3V3, its first end connects assist gas pipeline and unstrpped gas pipeline, its second end connects second end of first six-way valve, and its 3rd end connects the upper entrance end of fluid bed microreactor R2.Realized the switching of fixed-bed micro-reactor and fluid bed evaluation system unstrpped gas and gas assist gas like this, easily.
Further, the assist gas pipeline comprises: air pipe line 15, nitrogen pipeline 17 and the second triple valve 3V2, first end of the second triple valve 3V2 connects air pipe line 15, and its second end connects nitrogen pipeline 17, and its 3rd end is connected with first end of the 3rd triple valve 3V3.The air of air pipe line can derive from the air steel cylinder, and the nitrogen of nitrogen pipeline can derive from the nitrogen steel cylinder.On air pipe line or the nitrogen pipeline stop valve can be set, with gauge tap, for example the stop valve that is provided with on the nitrogen pipeline is ball valve BV3.In addition, also be provided with spinner flowmeter MC1 on the air inlet pipeline, it is arranged between the second triple valve 3V2 and the 3rd triple valve 3V3, and spinner flowmeter MC2 is arranged on the air pipe line 15 and is positioned at before the second triple valve 3V2, with control with observe flow.
Further, the raw material pipeline comprises: the first unstrpped gas pipeline 11, the second unstrpped gas pipeline 13 and the first triple valve 3V1, first end of the first triple valve 3V1 connects the first unstrpped gas pipeline 11, its second end connects other reaction gas pipeline 13, and its 3rd end is connected with first end of the 3rd triple valve 3V3.Can connect switching controls with various reacting gas easily by the first triple valve 3V1.
As shown in Figure 1, can realize the switching of fixed bed minisize reaction and fluidized-bed reaction by the switching of the 3rd triple valve 3V3 and the 6th triple valve 3V6 valve.When the 3rd triple valve 3V3 first end communicates with the 3rd triple valve 3V3 the 3rd end, when the 6th triple valve 3V6 first end communicates with the 6th triple valve 3V6 the 3rd end, the fluid bed microreactor is in running order.
When the 3rd triple valve 3V3 first end communicates with the 3rd triple valve 3V3 second end, when the 6th triple valve 3V6 first end communicates with the 6th triple valve 3V6 second end, fixed-bed micro-reactor is in running order.(dimethyl ether is through the first unstrpped gas pipeline 11, the 3rd triple valve 3V3, the first six-way valve 6V1 (is little anti-charging continuously when quantity tube 32 links to each other with five terminal with 6V1 second end, quantity tube 32 is the pulse micro-inverse charging when linking to each other with the 4th end with 6V1 the 3rd end), the second six-way valve 6V2, fixed-bed micro-reactor R1 carries out the fixed bed minisize reaction, then through the 6th triple valve 3V6, the second six-way valve 6V2 (quantity tube 33 is the pulse micro-inverse discharging when linking to each other with second end with 6V3 one end, is little anti-discharging continuously when quantity tube 32 links to each other with five terminal with 6V1 the 4th end), product gas enters chromatography to carry out quantitatively.
Switching by the 3rd triple valve 3V3 and the 6th triple valve 3V6 valve can be switched fixed bed minisize reaction and fixed fluidized bed reaction, realized being used for both can carrying out the fixed bed minisize reaction on the device of evaluating catalyst, also can carry out fixed fluidized bed reaction at a cover.
As shown in Figure 1, can realize the switching of assist gas in the catalytic reaction process easily by the switching of the second triple valve 3V2.When the 3rd end of the second triple valve 3V2 communicated with second end of the second triple valve 3V2, nitrogen entered fluid bed microreactor R2 through nitrogen gas circuit 17 by the second triple valve 3V2, the 3rd triple valve 3V3; By the second triple valve 3V2, the 3rd triple valve 3V3, the first six-way valve 6V1, the 4th triple valve 3V4, the second six-way valve 6V2 enters fixed-bed micro-reactor, and fixed-bed micro-reactor or fluid bed microreactor bed are in nitrogen and purge state.
When the 3rd end of the second triple valve 3V2 communicated with the first end air of the second triple valve 3V2, air entered the fluid bed microreactor through air gas circuit 15 by the second triple valve 3V2, the 3rd triple valve 3V3; By the second triple valve 3V2, the 3rd triple valve 3V3, the first six-way valve 6V1, the 4th triple valve 3V4, the second six-way valve 6V2 enters fixed-bed micro-reactor, and fixed-bed micro-reactor or fluid bed microreactor bed are in reproduced state.
As shown in Figure 1, realize the switching of catalytic reaction differential responses unstrpped gas by the switching of the first triple valve 3V1.When the first triple valve 3V1 and the first unstrpped gas pipeline 11, when for example the dimethyl ether pipeline communicates, dimethyl ether enters fluid bed microreactor R2 by the first triple valve 3V1, the 3rd triple valve 3V3, or through the first triple valve 3V1, the 3rd triple valve 3V3, the first six-way valve 6V1, the 4th triple valve 3V4, the second six-way valve 6V2 enters fixed-bed micro-reactor R1, and what carry out in fixed-bed micro-reactor or the fluid bed microreactor is the dimethyl ether catalysis cracking reaction.
When the first triple valve 3V1 communicated with the second unstrpped gas pipeline 13, second unstrpped gas entered fluid bed microreactor R2 through the second unstrpped gas pipeline 13 by the first triple valve 3V1, the 3rd triple valve 3V3; Or by the first triple valve 3V1, the 3rd triple valve 3V3, the first six-way valve 6V1, the 4th triple valve 3V4, the second six-way valve 6V2 enters fixed-bed micro-reactor R1, what carry out in fixed-bed micro-reactor or the fluid bed microreactor is the pairing reactions of other raw materials, for example the C during the higher hydrocarbons cracking reaction
4, C
5Or C
6The pairing reaction of 2-butylene gas when the pairing reaction of gas, isomerization reaction.
Further, the raw material pipeline also comprises: flow control system, and to realize accurate control to raw feed materials.Flow control system can be arranged on the diverse location of raw material pipeline.Further, the raw material pipeline also comprises: flow control system is connected between first end of the 3rd end of the first triple valve 3V1 and the 3rd triple valve 3V3.Like this, can all control the first unstrpped gas pipeline, reaction gas pipeline.Further, flow control system comprises: the pressure-reducing valve JV1 of series connection, magnetic valve PC, check valve DV and mass flowmenter MFC.Can realize quality control accurately to raw material pipeline feed, its control accuracy height by mass flowmenter MFC.
Further, as shown in Figure 2, fixed-bed micro-reactor R1 comprises: fixed-bed micro-reactor main body 20, its inner chamber are cavity, the gas vent 25 that carries out the fixed bed piston flow reactor, the liquid-inlet 21 that is arranged on fixed-bed micro-reactor main body 20 tops and gas access 23.Liquid charging stock enters in the fixed-bed micro-reactor R1 inner chamber by liquid-inlet 21, and gas raw material enters in the fixed-bed micro-reactor R1 inner chamber by gas access 23.Liquid-inlet 21 and gas access 23 are arranged on fixed-bed micro-reactor R1 top.This reactor can be realized gas raw material or liquid charging stock sample introduction, pulse or continuous sample introduction.
Further, liquid-inlet 21 is arranged on the top of fixed-bed micro-reactor main body 20, and gas access 23 is arranged on the side of fixed-bed micro-reactor main body 20, and gas vent 25 is arranged on the bottom of fixed-bed micro-reactor main body 20.Liquid-inlet 21, gas access 23 and gas vent 25 are separately positioned on the two ends and the side of fixed-bed micro-reactor main body 20, and charging, discharging route are reasonable, are independent of each other, and help being maintained fixed an intensity of microreactor main body 20.
Further, fixed-bed micro-reactor R1 also comprises: spiro union portion 22, and for example it has external screw thread, is set in fixed-bed micro-reactor main body 20 upper ends by welding; Seal cover 26, for example it is a silicagel pad, or other elastic sealing gaskets, be arranged on the end of spiro union portion 22 and the cavity of sealing and fixing bed microreactor main body 20, syringe 211 passes seal cover 26, and liquid-inlet 21 is arranged on the syringe 211, for example, liquid-inlet 21 is arranged in the injection canal of syringe 211; Clamp nut 24 is spirally connected with spiro union portion 22 and is pressed on outside the seal cover 26, and for example clamp nut 24 is for having the clamp nut of internal thread, and syringe 211 passes seal cover 26.The mode of reactor bottom by syringe 211 chargings goed deep in fixed-bed micro-reactor R1 employing from the top, make liquid charging stock, after for example methyl alcohol comes out from syringe 211, contact with the beds of constant temperature zone in reactor top preheating gasification back, low dose of liquid charging stock can be used, the use amount of liquid charging stock can be accurately calculated.Syringe can adopt manual injector, also can adopt the automatic feed pump.
The fluid bed microreactor carries out the moulding catalyst performance evaluation or carries out optimization of process conditions, and reaction unit design is complicated, and cost is higher, and catalyst and raw material requirement are bigger.This device adopts the small-sized fluidized bed microreactor that preformed catalyst is estimated, and can only can satisfy the investigation fluidization conditions with little amount of catalyst not possessing under the catalyst amplification condition, realizes the test to the preformed catalyst performance.This installs flexible design, and is easy and simple to handle, saves raw material.
The invention also discloses a kind of method that is used for evaluating catalyst, use the foregoing device that is used for evaluating catalyst, realize the evaluations of fixed-bed micro-reactor evaluation and fluid bed microreactor.This method that is used for evaluating catalyst is used a cover air inlet pipeline and a raw material pipeline, can estimate the catalytic performance of catalyst activity component such as molecular sieve catalytic performance or preformed catalyst respectively as required.The fluid bed microreactor has reduced cost, and flexible operation is reliable.
Further, be used for the method for evaluating catalyst, fixed-bed micro-reactor adopts manual charging or adopts automatic feed.Further, fixed-bed micro-reactor is for example clicked six-way valve 6V1 by valve control system, and manually charging is by magnetic valve PC automatic feed.
Further, fluid bed microreactor automatic feed.Further, the fluid bed microreactor passes through the valve control system automatic feed, for example, and by magnetic valve PC automatic feed.
The concrete course of work of the present invention is described below
1, fixed bed pulse minisize reaction catalyst compressing tablet, screening 20～40 order particles are used for catalyst performance evaluation.Take by weighing the 200mg catalyst, among the fixed-bed micro-reactor R1 that packs into (being called for short reactor R1), upper and lower silica wool and the quartz sand of being equipped with respectively of beds.Reactor R1 is packed among the fixed bed heating furnace HT1 into coupled reaction device R1 inlet, outlet line.Open N
2Steel cylinder is (with N
2Gas circuit 17 connects) main valve and stop valve BV3,3V2 switches to N with triple valve
2Gas circuit 17 1 sides.Setting spinner flowmeter MC1 flow is 30ml/min.Six-way valve 6V1,6V2,6V3 are switched to the position that N2 enters reactor R1, the check system air-tightness.
With triple valve 3V6 incision fixed-bed micro-reactor one side.Setting fixed bed heating furnace HT1 is 500 ℃.HT1 controls according to temperature programming with the fixed bed heating furnace, at 500 ℃ of following N
2Purge beds 1h, program is set to 450 ℃ of reaction temperatures with fixed bed heating furnace HT1 temperature automatically, keeps certain hour under this temperature.Close stop valve (ball valve) BV3, open stop valve (ball valve) BV1, triple valve 3V1 is switched to the state that links to each other with dimethyl ether gas circuit (being equivalent to the first unstrpped gas pipeline 11).According to the flow value of test space velocity conditions setting mass flowmenter MFC, set dilution N according to actual needs
2The flow value of spinner flowmeter is clicked magnetic valve PC.The quantity tube 32 of six-way valve 6V1 is communicated with the left side first unstrpped gas pipeline 11, and triple valve 3V4 is in the position of emptying, and six-way valve 6V2 switches to the state of charging, six-way valve 6V3 is switched on the pipeline position of quantity tube 33 samplings.Click six-way valve 6V1 and begin the pulse charging, the product gas in the six-way valve 6V3 quantity tube 33 enters the chromatographic analysis system 30 (abbreviation chromatogram) that is attached thereto.
After collection analysis of chromatogram is finished, repeat the multiple pulses charging.After pulse fixed bed minisize reaction is finished, stop motor-driven valve PC, close stop valve (ball valve) BV1.Reactor R1 temperature is set at room temperature, opens stop valve (ball valve) BV3, change the flow of spinner flowmeter MC1 into 30ml/min, use N
2Behind blow line, the beds certain hour, finished catalyst fixed bed minisize reaction evaluation.
As need catalyst is carried out in-situ regeneration, can be at N
2After purging is finished, triple valve 3V2 is switched to air gas circuit 17 1 sides, carry out the in-situ regeneration of catalyst, can repeat reaction-regenerative operation at 600 ℃ of blowing airs.
The pulse charging both can realize the gas of dimethyl ether charging, also can adopt manual methyl alcohol pulse charging by syringe 211.Adopt formerly chromatogram to carry out the quantitative analysis product gas.
2, the continuous minisize reaction of fixed bed
The catalyst compressing tablet, screening 20～40 order particles are used for catalyst performance evaluation.Take by weighing the 200mg catalyst, among the microreactor R1 that packs into, upper and lower silica wool and the quartz sand of being equipped with respectively of beds.Reactor R1 is packed among the fixed bed heating furnace HT1 into coupled reaction device R1 inlet, outlet line.Open N
2Steel cylinder main valve and stop valve (ball valve) BV3,3V2 switches to N with triple valve
2Gas circuit one side.Setting the spinner flowmeter flow is 30ml/min.Six-way valve 6V1,6V2,6V3 are switched to N
2Enter the position of reactor R1, the check system air-tightness.
With triple valve 3V6 incision fixed-bed micro-reactor R1 one side.Setting fixed bed heating furnace HT1 is 500 ℃.HT1 controls according to temperature programming with the fixed bed heating furnace, at 500 ℃ of following N
2Purge beds 1h, program is set to 450 ℃ of reaction temperatures with heating furnace HT1 temperature automatically, keeps certain hour under this temperature.Close stop valve (ball valve) BV3, open stop valve (ball valve) BV1, triple valve 3V1 is switched to the state that links to each other with the dimethyl ether gas circuit.According to the flow value of test space velocity conditions setting mass flowmenter MFC, set dilution N according to actual needs
2The flow value of spinner flowmeter is clicked magnetic valve PC.The quantity tube 32 of six-way valve 6V1 is linked to each other with right side carrier gas 35, and triple valve 3V4 is in the position of emptying, and six-way valve 6V2 switches to the state of charging, and six-way valve 6V3 is switched on the emptying position.Gather product gas with the gas collection bag from 6V3 emptying every the set time, the product gas of collecting in the gas collection bag is connected with off-line injection port 31, carry out the off-line quantitative analysis.
After the fixed bed minisize reaction is finished continuously, stop motor-driven valve PC, close stop valve (ball valve) BV1, set the MF1 flow and count 0.Temperature of reactor is set at room temperature, opens stop valve (ball valve) BV3, change the flow of spinner flowmeter into 30ml/min, N
2Behind blow line, the beds certain hour, finished catalyst fixed bed minisize reaction evaluation.
3, fluid bed evaluation
The 0.2g preformed catalyst pack in fluid bed microreactor R2, reactor is packed among the fluidized bed furnace HT2, connect pipeline.Open N
2The steel cylinder main valve, reconciling the decompression downstream pressure is 0.35Mpa, ball valve BV3 switches to N
2In the gas circuit, triple valve 3V6 switches to fluid bed microreactor R2, and triple valve 3V5 switches to into six-way valve 6V2, and six-way valve 6V3 switches to the position that quantity tube 33 links to each other with blow-down pipe, regulates N
2The spinner flowmeter flow value is 30ml/min, the check system air-tightness.
Fluid bed microreactor heating furnace begins to heat up.After treating that fluid bed minisize reaction actuator temperature reaches 500 ℃, regulating the spinner flowmeter flow is 30ml/min, N
2Purge beds 1h continuously.After purging the bed end, fluid bed microreactor heating furnace enters temperature-fall period, bed temperature drops to 450 ℃ from 500 ℃, treat that bed temperature is behind 450 ℃ of stable 30min, open ball valve BV1, triple valve 3V1 is linked in dimethyl ether gas circuit or other reacting gas gas circuits,, regulate diluent gas N by spinner flowmeter according to the flow of air speed setting mass flowmenter MFC
2Flow is clicked magnetic valve PC.System begins to advance continuously the unstripped gas dimethyl ether, according to the time of program setting, behind charging 5min, clicks " beginning " key of chromatographic analysis system 30, and six-way valve 6V3 samples automatically, chromatography product gas.
After system gathered first sample automatically, (suggestion 5min gathers a gas phase sample) gathered the gas phase sample at six-way valve 6V3 emptying place off-line at regular intervals at interval, prepares off-line analysis.(being generally 30min) after continuous feed is finished, stopping motor-driven valve PC, is 0 with the spinner flowmeter flow set.Temperature of reactor is set at room temperature, reconciles N
2The flow value of spinner flowmeter is 30ml/min, and purging system, bed begin cooling.
As need catalyst is carried out in-situ regeneration, can be at N
2After purging is finished, triple valve 3V2 is switched to air one side, carry out the in-situ regeneration of catalyst, can repeat reaction-regenerative operation at 600 ℃ of blowing airs.
As can be seen from the above description, the above embodiments of the present invention have realized following technique effect:
The present invention has the characteristics of applied range, and it is applicable to the evaluating catalyst of differential responses system.Go for normal pressure or compressive reaction system.Fixed-bed micro-reactor both can adopt gas-phase feed, also can adopt the mode of liquid phase feeding; Can realize screening of catalyst, also can be used for kinetics or the dynamic (dynamical) research of carbon distribution inactivation reaction.The fluid bed microreactor can be investigated the catalytic performance of catalyst under fluidized state under the less condition of loaded catalyst.The present invention have operate steadily, the outstanding advantage of rational in infrastructure, diverse in function, help improving catalyst development efficient.
The above is the preferred embodiments of the present invention only, is not limited to the present invention, and for a person skilled in the art, the present invention can have various changes and variation.Within the spirit and principles in the present invention all, any modification of being done, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (17)
1. a device that is used for evaluating catalyst is characterized in that, comprising:
The assist gas pipeline;
The unstrpped gas pipeline;
Fixed-bed micro-reactor (R1) is connected with described unstrpped gas pipeline with described assist gas pipeline;
Fixed-bed micro-reactor heating furnace (HT1) heats described fixed-bed micro-reactor (R1);
Fluid bed microreactor (R2) is connected with described assist gas pipeline, described unstrpped gas pipeline, and with the shared identical outlet line of described fixed-bed micro-reactor (R1);
Fluid bed microreactor heating furnace (HT2) heats described fluid bed microreactor (R2).
2. the device that is used for evaluating catalyst according to claim 1 is characterized in that, also comprises:
Valve control system;
Described fixed-bed micro-reactor (R1) is connected with described unstrpped gas pipeline with described assist gas pipeline by described valve control system;
Described fluid bed microreactor (R2) is connected with described assist gas pipeline, described unstrpped gas pipeline, described fixed-bed micro-reactor (R1) the product gas port of export by described valve control system.
3. the device that is used for evaluating catalyst according to claim 2, it is characterized in that described valve control system comprises: first six-way valve (6V1), second six-way valve (6V2), the 3rd six-way valve (6V3), the 4th triple valve (3V4), the 5th triple valve (3V5); The device of described evaluating catalyst also comprises: first quantity tube (32);
Described first six-way valve (6V1), its first end connects the carrier gas interface from gas-chromatography, its the 3rd end connects described assist gas pipeline and described unstrpped gas pipeline, its the 4th end is connected with first end of described the 4th triple valve (3V4), its the 6th end is connected with first end of described second six-way valve (6V2), and second end of described first six-way valve (6V1), five terminal are connected with described first quantity tube (32) respectively;
Second end of described the 4th triple valve (3V4) is the first emptying end, and the 3rd end of described the 4th triple valve (3V4) connects the 3rd end of described second six-way valve (6V2);
Second end of described second six-way valve (6V2) connects the inlet of described fixed-bed micro-reactor (R1), and its five terminal connects the outlet line of described fixed-bed micro-reactor (R1) and fluid bed microreactor (R2).
Described the 3rd six-way valve (6V3), its first end connects the carrier gas from gas-chromatography, its second end connects the 6th end of described second six-way valve (6V2), the 3rd end, the 6th end of described the 3rd six-way valve (6V3) link to each other with quantity tube, its the 4th end connects the 4th end of the second six-way valve 6V2, and its five terminal is the second emptying end.
4. the device that is used for evaluating catalyst according to claim 2 is characterized in that,
Described valve control system also comprises: the 5th triple valve (3V5), the 4th end of described the 3rd six-way valve connects the 4th end of described second six-way valve (6V2) by first end of described the 5th triple valve (3V5), connect the 4th end of described second six-way valve (6V2) by second end of described the 5th triple valve (3V5), the 3rd end of described the 5th triple valve (3V5) is off-line gas sampling mouth (31) or calibrating gas injection port.
5. the device that is used for evaluating catalyst according to claim 4 is characterized in that,
Described first six-way valve (6V1) is pneumatic control formula six-way valve or electronic control formula six-way valve.
6. the device that is used for evaluating catalyst according to claim 5 is characterized in that,
Described the 3rd six-way valve (6V3) is pneumatic control formula six-way valve or electronic control formula six-way valve.
7. the device that is used for evaluating catalyst according to claim 6 is characterized in that,
Also comprise: the 3rd triple valve (3V3), its first end connect described assist gas pipeline and described unstrpped gas pipeline, and its second end connects second end of described first six-way valve, and its 3rd end connects the arrival end on described fluid bed microreactor (R2) top.
8. the device that is used for evaluating catalyst according to claim 7 is characterized in that,
Described assist gas pipeline comprises: air pipe line, nitrogen pipeline and second triple valve (3V2), first end of described second triple valve (3V2) connects described air pipe line, its second end connects described nitrogen pipeline, and its 3rd end is connected with first end of described the 3rd triple valve (3V3) through spinner flowmeter (MC1).
9. the device that is used for evaluating catalyst according to claim 8 is characterized in that,
Described unstrpped gas pipeline comprises: the first unstrpped gas pipeline, the second unstrpped gas pipeline and first triple valve (3V1), first end of described first triple valve (3V1) connects the described first unstrpped gas pipeline, its second end connects the described second unstrpped gas pipeline, and its 3rd end is connected with first end of described the 3rd triple valve (3V3).
10. the device that is used for evaluating catalyst according to claim 9 is characterized in that,
Described unstrpped gas pipeline also comprises: flow control system.
11. the device that is used for evaluating catalyst according to claim 10 is characterized in that,
Described flow control system is connected between first end of the 3rd end of described first triple valve (3V1) and described the 3rd triple valve (3V3).
12. the device that is used for evaluating catalyst according to claim 11 is characterized in that,
Described flow control system comprises: Chuan Lian pressure-reducing valve (JV1), magnetic valve (PC), check valve (DV1) and mass flowmenter (MFC) successively, wherein, the preceding check valve (DV1) that is provided with of described mass flowmenter (MFC).
13. the device that is used for evaluating catalyst according to claim 12 is characterized in that,
Described fixed-bed micro-reactor (R1) comprising: fixed-bed micro-reactor main body (20), gas vent (25), the liquid-inlet (21) that is arranged on described fixed-bed micro-reactor main body (20) top and gas access (23).
14. the device that is used for evaluating catalyst according to claim 13 is characterized in that,
Described liquid-inlet (21) is arranged on the top of described fixed-bed micro-reactor main body (20), described gas access (23) is arranged on the side of described fixed-bed micro-reactor main body (20), and described gas vent (25) is arranged on the bottom of described fixed-bed micro-reactor main body (20).
15. the device that is used for evaluating catalyst according to claim 14 is characterized in that,
Described fixed-bed micro-reactor (R1) also comprises: spiro union portion (22) is set in described fixed-bed micro-reactor main body (20) upper end and has external screw thread; Seal cover (26) is arranged on the end of described spiro union portion (22) and seals the cavity of described fixed-bed micro-reactor main body (20); Syringe (211) passes described seal cover (26), and described syringe (211) is provided with described liquid-inlet (21); Clamp nut is with the external thread bolt connection of described spiro union portion (22) and be pressed on the described seal cover (26).
16. a method that is used for evaluating catalyst is characterized in that, uses each described device that is used for evaluating catalyst in the claim 1 to 15, and fixed-bed micro-reactor adopts manual charging or adopts automatic feed.
17. the method that is used for evaluating catalyst according to claim 16 is characterized in that, the automatic feed of fluid bed microreactor.
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| CN102539618B (en) * | 2012-01-10 | 2015-02-25 | 北京昊诚油气科技有限公司 | Multi-channel high-throughput catalyst evaluation device and evaluation method |
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