CN101905139B - Device and method for evaluating catalyst - Google Patents
Device and method for evaluating catalyst Download PDFInfo
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- CN101905139B CN101905139B CN2010102288551A CN201010228855A CN101905139B CN 101905139 B CN101905139 B CN 101905139B CN 2010102288551 A CN2010102288551 A CN 2010102288551A CN 201010228855 A CN201010228855 A CN 201010228855A CN 101905139 B CN101905139 B CN 101905139B
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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 evaluating catalyst system investment height, problems such as complicated operation.Through 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, a kind of device that is used for evaluating catalyst is provided, has 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 through valve control system; The fluid bed microreactor is connected with assist gas pipeline, unstrpped gas pipeline, fixed-bed micro-reactor export pipeline through 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 connects the inlet of fixed-bed micro-reactor, 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 4th end is through 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 through first end of the 5th triple valve; Connect the 4th end of second six-way valve through 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 and the 3rd triple valve of first 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 said 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 with 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 explaining 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 characteristic among the embodiment among the application can make up each other.Below with reference to accompanying drawing and combine embodiment to specify the present invention.
As shown in Figure 1, comprise according to the device that is used for evaluating catalyst of the embodiment of the invention: 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 through temperature-control heat couple is set, and to obtain suitable reaction temperature, measure the temperature of reactor diverse location through 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; Air inlet pipeline comprises that the gas that is used to dilute unstrpped gas, post catalyst reaction bed when being used for beds activation, purging, 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 with 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 through valve control system; Fluid bed microreactor R2 is connected with assist gas pipeline, unstrpped gas pipeline, fixed bed minisize reaction export pipeline through valve control system.This valve control system can be made up of a plurality of valves, to realize that each stage of valve control system is controlled air feed and confession raw material.Can realize the switching of fixed-bed micro-reactor and fluid bed microreactor through 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; Simplify the connection of equipment, reduced 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, 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 3V4; Its 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 connects the inlet of fixed-bed micro-reactor R1, and its five terminal connects the outlet line of fixed-bed micro-reactor 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 gets into chromatographic analysis system 30 injection ports, and its second end connects the 6th end of the second six-way valve 6V2, and its 4th end connects the 4th end of the second six-way valve 6V2 through 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.
Through 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, thus 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 practiced thrift 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 through first end of the 5th triple valve 3V5; Connect the 4th end of the second six-way valve 6V2 through 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, the stop valve that for example 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 the switching controls with various reacting gas easily through the first triple valve 3V1.
As shown in Figure 1, can realize the switching of fixed bed minisize reaction and fluidized-bed reaction through 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 little anti-charging continuously through the first unstrpped gas pipeline 11, the 3rd triple valve 3V3, the first six-way valve 6V1 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; Get into chromatography and carry out quantitatively 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 then.
Switching through 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 through 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 got into fluid bed microreactor R2 through nitrogen gas circuit 17 through the second triple valve 3V2, the 3rd triple valve 3V3; Through 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 gets into 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 got into the fluid bed microreactor through air gas circuit 15 through the second triple valve 3V2, the 3rd triple valve 3V3; Through 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 gets into 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 through 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 gets into fluid bed microreactor R2 through 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 gets into 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 got into fluid bed microreactor R2 through the second unstrpped gas pipeline 13 through 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 gets into 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 and the 3rd triple valve 3V3 of the first triple valve 3V1.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 the quality control accurately to raw material pipeline feed through mass flowmenter MFC, its control accuracy is high.
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 gets in the fixed-bed micro-reactor R1 inner chamber through liquid-inlet 21, and gas raw material gets in the fixed-bed micro-reactor R1 inner chamber through gas access 23.Liquid-inlet 21 is arranged on fixed-bed micro-reactor R1 top with gas access 23.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 keeping the intensity of fixed-bed micro-reactor 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 through 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 through 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; Preheating gasification back contacts with the beds of constant temperature zone on reactor top, can use low dose of liquid charging stock, can accurately calculate the use amount of liquid charging stock.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 through valve control system, and manually charging is through 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 through 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 gets into reactor R1, 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, under this temperature, keeps certain hour.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 according to actual needs and use N
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 gets into the chromatographic analysis system 30 (abbreviation chromatogram) that is attached thereto.
After collection analysis of chromatogram is accomplished, repeat the multiple pulses charging.Pulse fixed bed minisize reaction stops motor-driven valve PC after accomplishing, and closes 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, accomplished catalyst fixed bed minisize reaction evaluation.
Like need catalyst is carried out in-situ regeneration, can be at N
2After purge accomplishing, 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 through 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
2Get into 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, under this temperature, keeps certain hour.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 according to actual needs and use N
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.Every separated set time is gathered product gas with the gas collection bag from 6V3 emptying, and the product gas of collecting in the gas collection bag is connected with off-line injection port 31, carries out the off-line quantitative analysis.
After the fixed bed minisize reaction is accomplished 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, accomplished 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 gets into temperature-fall period, and bed temperature drops to 450 ℃ from 500 ℃, treats 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 through 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.After continuous feed is accomplished (being generally 30min), 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.
Like need catalyst is carried out in-situ regeneration, can be at N
2After purge accomplishing, 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.
From above description, can find out that 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 merely the preferred embodiments of the present invention, is not limited to the present invention, and for a person skilled in the art, the present invention can have various changes and variation.All within spirit of the present invention and principle, any modification of being done, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (16)
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 said unstrpped gas pipeline with said assist gas pipeline;
Fixed-bed micro-reactor heating furnace (HT1) heats said fixed-bed micro-reactor (R1);
Fluid bed microreactor (R2) is connected with said assist gas pipeline, said unstrpped gas pipeline, and with the shared identical outlet line of said fixed-bed micro-reactor (R1);
Fluid bed microreactor heating furnace (HT2) heats said fluid bed microreactor (R2);
Said fixed-bed micro-reactor heating furnace (HT1) and fluid bed microreactor heating furnace (HT2) carry out the temperature control heating through temperature-control heat couple is set;
Valve control system;
Said fixed-bed micro-reactor (R1) is connected with said unstrpped gas pipeline with said assist gas pipeline through said valve control system;
Said fluid bed microreactor (R2) is connected with said assist gas pipeline, said unstrpped gas pipeline, said fixed-bed micro-reactor (R1) the product gas port of export through said valve control system.
2. the device that is used for evaluating catalyst according to claim 1; It is characterized in that said 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 said evaluating catalyst also comprises: first quantity tube (32);
Said first six-way valve (6V1); Its first end connects the carrier gas interface from gas-chromatography; Its 3rd end connects said assist gas pipeline and said unstrpped gas pipeline; Its 4th end is connected with first end of said the 4th triple valve (3V4), and its 6th end is connected with first end of said second six-way valve (6V2), and second end of said first six-way valve (6V1), five terminal are connected with said first quantity tube (32) respectively;
Second end of said the 4th triple valve (3V4) is the first emptying end, and the 3rd end of said the 4th triple valve (3V4) connects the 3rd end of said second six-way valve (6V2);
Second end of said second six-way valve (6V2) connects the inlet of said fixed-bed micro-reactor (R1), and its five terminal connects the outlet line of said fixed-bed micro-reactor (R1) and fluid bed microreactor (R2).
Said the 3rd six-way valve (6V3); Its first end connects the carrier gas from gas-chromatography; Its second end connects the 6th end of said second six-way valve (6V2); The 3rd end, the 6th end of said the 3rd six-way valve (6V3) link to each other with quantity tube, and its 4th end connects the 4th end of second six-way valve (6V2), and its five terminal is the second emptying end.
3. the device that is used for evaluating catalyst according to claim 2; It is characterized in that; Said valve control system also comprises: the 5th triple valve (3V5); The 4th end of said the 3rd six-way valve connects the 4th end of said second six-way valve (6V2) through first end of said the 5th triple valve (3V5); Connect the 4th end of said second six-way valve (6V2) through second end of said the 5th triple valve (3V5), the 3rd end of said the 5th triple valve (3V5) is off-line gas sampling mouth (31) or calibrating gas injection port.
4. the device that is used for evaluating catalyst according to claim 3 is characterized in that, said first six-way valve (6V1) is pneumatic control formula six-way valve or electronic control formula six-way valve.
5. the device that is used for evaluating catalyst according to claim 4 is characterized in that, said the 3rd six-way valve (6V3) 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; It is characterized in that; Also comprise: the 3rd triple valve (3V3); Its first end connects said assist gas pipeline and said unstrpped gas pipeline, and its second end connects second end of said first six-way valve, and its 3rd end connects the arrival end on said fluid bed microreactor (R2) top.
7. the device that is used for evaluating catalyst according to claim 6; It is characterized in that; Said assist gas pipeline comprises: air pipe line, nitrogen pipeline and second triple valve (3V2); First end of said second triple valve (3V2) connects said air pipe line, and its second end connects said nitrogen pipeline, and its 3rd end is connected with first end of said the 3rd triple valve (3V3) through spinner flowmeter (MC1).
8. the device that is used for evaluating catalyst according to claim 7; It is characterized in that; Said unstrpped gas pipeline comprises: the first unstrpped gas pipeline, the second unstrpped gas pipeline and first triple valve (3V1); First end of said first triple valve (3V1) connects the said first unstrpped gas pipeline, and its second end connects the said second unstrpped gas pipeline, and its 3rd end is connected with first end of said the 3rd triple valve (3V3).
9. the device that is used for evaluating catalyst according to claim 8 is characterized in that, said unstrpped gas pipeline also comprises: flow control system.
10. the device that is used for evaluating catalyst according to claim 9 is characterized in that, said flow control system is connected between first end of the 3rd end and said the 3rd triple valve (3V3) of said first triple valve (3V1).
11. the device that is used for evaluating catalyst according to claim 10; It is characterized in that; Said flow control system comprises: pressure-reducing valve (JV1), magnetic valve (PC), check valve (DV1) and the mass flowmenter (MFC) of connecting successively; Wherein, the preceding check valve (DV1) that is provided with of said mass flowmenter (MFC).
12. the device that is used for evaluating catalyst according to claim 11; It is characterized in that said fixed-bed micro-reactor (R1) comprising: fixed-bed micro-reactor main body (20), gas vent (25), the liquid-inlet (21) that is arranged on said fixed-bed micro-reactor main body (20) top and gas access (23).
13. the device that is used for evaluating catalyst according to claim 12; It is characterized in that; Said liquid-inlet (21) is arranged on the top of said fixed-bed micro-reactor main body (20); Said gas access (23) is arranged on the side of said fixed-bed micro-reactor main body (20), and said gas vent (25) is arranged on the bottom of said fixed-bed micro-reactor main body (20).
14. the device that is used for evaluating catalyst according to claim 13 is characterized in that, said fixed-bed micro-reactor (R1) also comprises: spiro union portion (22) is set in said fixed-bed micro-reactor main body (20) upper end and has external screw thread; Seal cover (26) is arranged on the end of said spiro union portion (22) and seals the cavity of said fixed-bed micro-reactor main body (20); Syringe (211) passes said seal cover (26), and said syringe (211) is provided with said liquid-inlet (21); Clamp nut is with the external thread bolt connection of said spiro union portion (22) and be pressed on the said seal cover (26).
15. 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 14, and fixed-bed micro-reactor adopts manual charging or adopts automatic feed.
16. the method that is used for evaluating catalyst according to claim 15 is characterized in that, the automatic feed of fluid bed microreactor.
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| CN110270278B (en) * | 2019-06-27 | 2021-06-01 | 华北理工大学 | Sleeve reaction device |
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