CN107703251A - A kind of catalyst test apparatus and method - Google Patents

A kind of catalyst test apparatus and method Download PDF

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Publication number
CN107703251A
CN107703251A CN201711175218.0A CN201711175218A CN107703251A CN 107703251 A CN107703251 A CN 107703251A CN 201711175218 A CN201711175218 A CN 201711175218A CN 107703251 A CN107703251 A CN 107703251A
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catalyst
reactor
valve
product
reaction
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CN201711175218.0A
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田洪芹
王广亮
梁尚丛
冯川
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Kymson Luoyang Petrochemical Equipment Co ltd
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Luoyang Kai Meisheng Petrochemical Equipment Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N31/00Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
    • G01N31/10Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using catalysis

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Molecular Biology (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
  • Biochemistry (AREA)
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Abstract

The invention discloses a kind of catalyst test apparatus and method, the device includes steam generating system, source material delivery system, heater, reactor, reaction product collector, knockout drum and fume-dehydrating tank, utilize the device, after first will be water and raw material be mixed into heater, and mixed material enters in reactor after heating, and is sprayed by nozzle atomization, with the abundant haptoreaction of catalyst in reactor, reaction product is discharged from reactor head enters knockout drum through supercooling;Catalyst regeneration is carried out after reaction under certain condition, to gaseous product, product liquid and flue gas are collected and evaluated.Because the apparatus structure of the present invention is reasonable in design, atomizing raw materials effect is good, can truly reflect catalyst reaction performance, conversion ratio, yield, the performance such as the activity of catalyst, carbon distribution, selectivity, and operating process is simple, and cost is low.

Description

A kind of catalyst test apparatus and method
Technical field
The present invention relates to evaluating catalyst technical field, more particularly to a kind of catalyst test apparatus and method.
Background technology
Catalyst is catalyst important in chemical industry, and catalyst is the dynamic of promotion technology development in a sense Power, and the power to increase productivity.Catalyst performance evaluation device is that catalyst activity and selectivity is evaluated, to original The device that material conversion ratio, yield etc. are investigated, tank reactor are to carry out laboratory catalytic agent exploitation to pellet type catalyst And the device of performance evaluation, when being evaluated using tank reactor evaluating apparatus catalyst performance, by Catalyst packing After entering tank reactor, reaction condition is adjusted, reaction raw materials are introduced into tank reactor, collecting reaction product, product carried out Analysis;The parameters such as the specific surface area of catalyst are detected after the reaction was completed, and then realized to catalytic activity and selection The evaluation of property.
For the more real performance of evaluation catalyst, make the catalyst performance that evaluates true and reliable, closer to pass The performance that catalyst can show when application, effective improvement, Chinese patent have also been carried out to catalyst performance evaluation device 201010228855.1 disclosing the apparatus and method for evaluating catalyst, catalyst test apparatus is overcome to be only capable of to single The defects of catalyst of a certain reaction system is evaluated, fixed-bed micro-reactor and fluid bed microreactor are combined Together, operating efficiency is improved.
In the prior art, it is by a mother tube that reaction raw materials, which enter reactor, contacts and is reacted with catalyst, and Raw material is not atomized and is distributed so that contact of the raw material with catalyst is not abundant enough, influences reaction raw materials in catalyst In distribution, expanding, mass transfer and reaction, it is impossible to reflect and obtain truth when raw material and Catalyst are applied, also can not The reactivity worth of real reflection raw material, conversion ratio, yield, situations such as the activity of catalyst, carbon distribution, selectivity and life-span.Together When, existing catalyst test apparatus efficiency is low, and complicated, technical process is cumbersome, and use has inconvenience more.
The content of the invention
It is an object of the invention to overcome in the prior art atomizing raw materials effect it is poor, it is impossible to real reflection catalyst and original The performance of material, efficiency is low, complicated, and technique is cumbersome, the defects of evaluation result inaccuracy, proposes a kind of catalyst test apparatus And method, the device is compared with prior art, simple in construction, easy to operate, and atomizing raw materials effect is good, can truly reflect catalyst The performance such as reactivity worth, conversion ratio, yield, the activity of catalyst, carbon distribution, selectivity.
The object of the invention to solve the technical problems is realized using following technical scheme.Itd is proposed according to the present invention A kind of catalyst test apparatus, including water pot, steam generator, head tank, heater, reactor, reaction product collector, Fume-dehydrating tank, knockout drum;The water pot is connected with steam generator by water pump, steam generator and head tank with The arrival end connection of heater, is also associated with raw material pump between head tank and the arrival end of heater;Steam and raw material are heating Device by feed line enters reactor after being mixed and heated, and the port of export of feed line one end and heater connects, separately In the intercalation reaction device of one end, one end that feed line is located in reactor is provided with nozzle;
The reactor bottom is provided with catalyst outlet, and reacting product outlet is provided with reactor top and catalyst enters Mouthful, wherein, entrance of the reacting product outlet also with reaction product collector is connected, the outlet of the reaction product collector and flue gas Drain sump and knockout drum are all connected with, and fume-dehydrating tank top is provided with exhanst gas outlet, and bottom is provided with wastewater outlet;Gas-liquid separation Tank top is provided with product gas outlet, and bottom is provided with liquid product outlet;
Outlet conduit, the pipeline towards fume-dehydrating tank, the pipe towards knockout drum of the reaction product collector Road, the intersection of three pipelines are provided with the first valve;Is provided with pipeline between first valve and fume-dehydrating tank Two valves, the 3rd valve is provided with the pipeline between first valve and knockout drum;
The catalyst test apparatus also includes nitrogen pipeline and the air line nitrogen pipeline and air line with adding The arrival end connection of hot device.
The object of the invention to solve the technical problems can be also applied to the following technical measures to achieve further.
Foregoing catalyst test apparatus, wherein, the nozzle is microatomization nozzle, bull atomizer, the spray of target formula One kind in mouth, double venturis in hybrid feed nozzle, wikipedia type nozzle.
Foregoing catalyst test apparatus, wherein, the feed line is inserted from the top of reactor or side or bottom Enter in reactor.
Foregoing catalyst test apparatus, wherein, the feed line passes through reaction product successively from reactor head In outlet, reactor top intercalation reaction device.
Foregoing catalyst test apparatus, wherein, it is additionally provided with cooling medium on the reaction product collector.
A kind of method that evaluating catalyst is carried out using above-mentioned catalyst test apparatus, is comprised the following steps:
(1) course of reaction:Open the first valve and the 3rd valve, close the second valve, start water pump, the water warp in water pot Water pump enters steam generator, and heater is mixed into the raw material from raw material pump after steam generator gasification, heated Mixed material after device heating enters inside reactor through feed line;
Catalyst enters in reactor from the catalyst inlet of reactor head, and mixed material sprays after nozzle atomization, Fully contact and react with the catalyst in reactor;Reacting product outlet discharge at the top of the reacted device of reaction product, enters Enter reaction product collector, after cooling medium cools down, reaction product enters knockout drum, and gaseous product is from knockout drum The product gas outlet discharge at top is collected, and product liquid is discharged from the liquid product outlet of gas-liquid separation pot bottom and carried out Collect;
(2) catalyst regeneration process:After course of reaction terminates, the 3rd valve is closed, opens the second valve, while open nitrogen Valve on gas pipeline, nitrogen is sent into reactor by nitrogen pipeline, reactor purged using nitrogen, Ran Houguan The valve closed on nitrogen pipeline, the valve on air line is opened, air is introduced into reactor by air line, is catalyzed Agent is regenerated, and 580~740 DEG C of regeneration temperature, regenerated flue gas is cooled down by reacting product outlet into reaction product collector, Subsequently into fume-dehydrating tank, flue gas is collected from exhanst gas outlet discharge, and waste water is discharged from wastewater outlet;
(3) catalyst and the analysis of raw material reactivity worth:Gaseous product, the liquid that course of reaction and regenerative process are obtained produce Thing and flue gas are analyzed, and draw the reactivity worth data of catalyst and raw material, the data are evaluated, draw catalyst and The reactivity worth of raw material.
Foregoing evaluating catalyst method, wherein, step (1) reactor operating pressure is 0.01~20.0MPa, reactor Operation temperature is 400~680 DEG C.
Foregoing evaluating catalyst method, wherein, step (1) reactor operating pressure is 0.1~15.0MPa, reactor Operation temperature is 420~650 DEG C.
Foregoing evaluating catalyst method, wherein, char length is 1.0~4.0min when step (2) regenerates, and top is absolute Pressure is 0.10~0.40Mpa.
By above-mentioned technical proposal, the advantages of the present invention are:
Atomizing raw materials effect is good compared with prior art by the present invention, simple in construction, and technical process is easy, can be truer The performances such as the reactivity worth of reflection and evaluation catalyst, conversion ratio, yield, the activity of catalyst, carbon distribution, selectivity, and into This is low, suitable for producing in batches and widely using.
Brief description of the drawings
Fig. 1 is the first structure diagram of the present invention;
Fig. 2 is second of structure diagram of the present invention;
Fig. 3 is the third structure diagram of the present invention.
【Component symbol explanation】
1:Water pot 2:Water pump 3:Steam generator 4:Head tank 5:Raw material pump 6:Heater
7:Reactor top 8:Reacting product outlet 9:Cooling medium 10:Reaction product collector
11:Catalyst inlet 12:Reactor 13:Nozzle 14:Catalyst outlet
15:Product gas outlet 16:Knockout drum 17:Feed line 18:Wastewater outlet
19:Fume-dehydrating tank 20:Exhanst gas outlet 21:Liquid product outlet 22:Nitrogen pipeline
23:Air line 24:First valve 25:Second valve 26:3rd valve
Embodiment
Further to illustrate the present invention to reach the technological means and effect that predetermined goal of the invention is taken, below in conjunction with Accompanying drawing and preferred embodiment, to according to a kind of catalyst test apparatus proposed by the present invention, its embodiment, structure, spy Sign and its effect, describe in detail as after.
Embodiment 1
A kind of catalyst test apparatus, including water pot 1, steam generator 3, head tank 4, heater 6, feed line 17, reactor 12, reaction product collector 10, fume-dehydrating tank 19, knockout drum 16, wherein, water pot 1 and steam generator 3 are connected by water pump 2, and the arrival end of steam generator 3 and head tank 4 with heater 6 is connected, and head tank 4 and heater 6 enter Mouth is also associated with raw material pump 5 between end;Steam and raw material are entered anti-after heater 6 is mixed and heated by feed line 17 Device 12 is answered, is provided with heater on reactor 12, the port of export of feed line one end and heater connects, and the other end is from anti- Answer at the top of device in intercalation reaction device, one end that feed line is located in reactor is provided with nozzle 13, and the nozzle 13 is atomization Nozzle;The bottom of reactor 12 is provided with catalyst outlet 14, and reacting product outlet 8 is provided with reactor top 7 and catalyst enters Mouth 11, wherein, entrance of the reacting product outlet 8 also with reaction product collector 10 is connected, and the reaction product collector 10 goes out Mouth is all connected with fume-dehydrating tank 19 and knockout drum 16, and the upper end of fume-dehydrating tank 19 is exhanst gas outlet 20, and lower end is waste water Outlet 18;The upper end of knockout drum 16 is product gas outlet 15, and lower end is liquid product outlet 21.Reaction product collector 10 On be additionally provided with cooling medium 9;
The outlet conduit of reaction product collector 10, towards the pipeline of fume-dehydrating tank 19, towards knockout drum 16 Pipeline, the intersection of three pipelines are provided with the first valve 24;On pipeline between first valve 24 and fume-dehydrating tank 19 The second valve 25 is provided with, the 3rd valve 26 is provided with the pipeline between first valve 24 and knockout drum 16;
The catalyst test apparatus also includes nitrogen pipeline 22 and air line 23, the nitrogen pipeline 22 and air line 23 Arrival end with heater 6 is connected.
The method of evaluating catalyst is carried out using the device includes three steps:Course of reaction, catalyst regeneration process, catalyst Process is analyzed with raw material reactivity worth, wherein, final step:Catalyst and raw material reactivity worth analysis process, using existing skill Art means are carried out, and course of reaction and catalyst regeneration process are carried out using technical scheme, are specially:
(1) course of reaction:The first valve 24 and the 3rd valve 26 are opened, closes the second valve 25, starts water pump 2, water pot In water enter steam generator 3 through water pump, steam generator gasification after with the raw material from raw material pump 5 be mixed into heating Device 6, the mixed material after heated device heating enter inside reactor through feed line 17;
Catalyst enters in reactor 12 from the catalyst inlet 11 of reactor head, and mixed material is after the atomization of nozzle 13 Spray, fully contact and react with the catalyst in reactor, the operating pressure of reactor is 1.0MPa, and operation temperature is 420℃;Reacting product outlet 8 at the top of the reacted device of reaction product is discharged, into reaction product collector 10, through cooling medium After 9 coolings, reaction product enters knockout drum 16, product gas outlet 15 row of the gaseous product from the top of knockout drum 16 Go out to be collected, product liquid is collected from the discharge of liquid product outlet 21 of the bottom of knockout drum 16;
(2) catalyst regeneration process:After course of reaction terminates, the 3rd valve 26 is closed, the second valve 25 is opened, beats simultaneously The valve on nitrogen pipeline 22 is opened, nitrogen is sent into reactor by nitrogen pipeline 22, reactor blown using nitrogen Sweep, the valve being then shut off on nitrogen pipeline, open the valve on air line, air is introduced into reaction by air line 23 Device, carry out catalyst regeneration, 580 DEG C, char length 1.0min, top absolute pressure 0.10Mpa of regeneration temperature, regenerated flue gas warp Cross reacting product outlet 8 to be cooled down into reaction product collector 10, subsequently into fume-dehydrating tank 19, flue gas goes out from flue gas The discharge of mouth 20 is collected, and waste water is discharged from wastewater outlet 18;
(3) catalyst and the analysis of raw material reactivity worth:Gaseous product, the liquid that course of reaction and regenerative process are obtained produce Thing and flue gas are analyzed, and draw the reactivity worth data of catalyst and raw material, the data are evaluated, draw catalyst and The reactivity worth of raw material.
Embodiment 2
Feed line is out of reactor bottom intercalation reaction device, and course of reaction reactor operating pressure is 20.0MPa, instead It is 680 DEG C to answer device operation temperature, 580 DEG C, char length 1.5min of catalyst regeneration temperature, top absolute pressure 0.10Mpa.Its It is the same as embodiment 1.
Embodiment 3
Feed line is out of reactor side intercalation reaction device, and course of reaction reactor operating pressure is 1.0MPa, instead It is 450 DEG C to answer device operation temperature, 580 DEG C, char length 4.0min of catalyst regeneration temperature, top absolute pressure 0.10Mpa.Its It is the same as embodiment 1.
Embodiment 4
Feed line is out of reactor side intercalation reaction device, and nozzle is microatomization nozzle, course of reaction reactor Operating pressure is 1.0MPa, and reactor operation temperature is 500 DEG C, 580 DEG C, char length 3.0min of catalyst regeneration temperature, top Portion absolute pressure 0.10Mpa.The other the same as in Example 1.
Embodiment 5
Feed line is out of reactor side intercalation reaction device, and nozzle is bull atomizer, course of reaction reactor Operating pressure is 1.0MPa, and reactor operation temperature is 650 DEG C, 740 DEG C, char length 2.0min of catalyst regeneration temperature, top Portion absolute pressure 0.40Mpa.The other the same as in Example 1.
Embodiment 6
For feed line out of reactor side intercalation reaction device, nozzle is target spray nozzle, and course of reaction reactor operates Pressure is 10.0MPa, and reactor operation temperature is 550 DEG C, and 640 DEG C, char length 2.0min of catalyst regeneration temperature, top is exhausted To pressure 0.2Mpa.The other the same as in Example 1.
Embodiment 7
For feed line out of reactor side intercalation reaction device, nozzle is hybrid feed nozzle in double venturis, is reacted Process reactor operating pressure is 15.0MPa, and reactor operation temperature is 600 DEG C, 660 DEG C of catalyst regeneration temperature, when burning Between 2.0min, top absolute pressure 0.20Mpa.
Embodiment 8
Feed line is out of reactor side intercalation reaction device, and nozzle is double wikipedia type nozzles, course of reaction reactor Operating pressure is 5.0MPa, and reactor operation temperature is 480 DEG C, 600 DEG C, char length 2.0min of catalyst regeneration temperature, top Portion absolute pressure 0.40Mpa.The other the same as in Example 1.
The above described is only a preferred embodiment of the present invention, not doing any formal limitation to the present invention, appoint What those skilled in the art, without departing from the scope of the present invention, is made a little using above-mentioned technology contents Change or the embodiment of modification, in the range of still falling within technical solution of the present invention.

Claims (9)

1. a kind of catalyst test apparatus, including water pot (1), steam generator (3), head tank (4), heater (6), reactor (12), reaction product collector (10), fume-dehydrating tank (19), knockout drum (16);It is characterized in that the water pot (1) with Steam generator (3) is connected by water pump (2), and the arrival end of steam generator (3) and head tank (4) with heater (6) connects Connect, raw material pump (5) is also associated between the arrival end of head tank (4) and heater (6);Steam and raw material are mixed in heater (6) Merge and reactor (12) is entered by feed line (17) after heating, feed line (17) one end goes out with heater (6) The connection of mouth end, other end intercalation reaction device (12) is interior, and one end that feed line is located in reactor is provided with nozzle (13);
Reactor (12) bottom is provided with catalyst outlet (14), and reacting product outlet (8) is provided with reactor top (7) With catalyst inlet (11), wherein, entrance of the reacting product outlet (8) also with reaction product collector (10) is connected, the reaction The outlet of product collector (10) is all connected with fume-dehydrating tank (19) and knockout drum (16), at the top of fume-dehydrating tank (19) Provided with exhanst gas outlet (20), bottom is provided with wastewater outlet (18);Product gas outlet (15) is provided with the top of knockout drum (16), Bottom is provided with liquid product outlet (21);
The outlet conduit of the reaction product collector (10), towards the pipeline of fume-dehydrating tank (19), towards knockout drum (16) pipeline, the intersection of three pipelines are provided with the first valve (24);First valve (24) and fume-dehydrating tank (19) Between pipeline on be provided with the second valve (25), set on the pipeline between first valve (24) and knockout drum (16) There is the 3rd valve (26);
The catalyst test apparatus also includes nitrogen pipeline (22) and air line (23), the nitrogen pipeline (22) and air hose Arrival end of the line (23) with heater (6) is connected.
2. catalyst test apparatus as claimed in claim 1, it is characterised in that the nozzle (13) is microatomization nozzle, more Head atomizer, target spray nozzle, one kind in double venturis in hybrid feed nozzle, wikipedia type nozzle.
3. catalyst test apparatus as claimed in claim 1, it is characterised in that the feed line (17) is from reactor (12) in top or side or bottom intercalation reaction device.
4. catalyst test apparatus as claimed in claim 1, it is characterised in that the feed line (17) is from reactor (12) top is successively by reacting product outlet (8), reactor top (7) intercalation reaction device.
5. catalyst test apparatus as claimed in claim 1, it is characterised in that also set on the reaction product collector (10) There is cooling medium (9).
A kind of 6. method that evaluating catalyst is carried out using catalyst test apparatus described in claim 1, it is characterised in that including Following steps:
(1) course of reaction:The first valve (24) and the 3rd valve (26) are opened, closes the second valve (25), starts water pump (2), Water in water pot enters steam generator (3) through water pump, is mixed after steam generator gasification with the raw material from raw material pump (5) Into heater (6), the mixed material after heated device heating enters inside reactor through feed line (17);
Catalyst enters in reactor (12) from the catalyst inlet (11) of reactor head, and mixed material is atomized through nozzle (13) After spray, fully contact and react with the catalyst in reactor;Reacting product outlet at the top of the reacted device of reaction product (8) discharge, into reaction product collector (10), after cooling medium (9) cooling, reaction product enters knockout drum (16), gaseous product is collected from product gas outlet (15) discharge at the top of knockout drum (16), and product liquid is from gas Liquid product outlet (21) discharge of liquid knockout drum (16) bottom is collected;
(2) catalyst regeneration process:After course of reaction terminates, the 3rd valve (26) is closed, the second valve (25) is opened, beats simultaneously The valve on nitrogen pipeline (22) is opened, nitrogen is sent into reactor by nitrogen pipeline (22), reactor entered using nitrogen Row purging, the valve being then shut off on nitrogen pipeline, opens the valve on air line, air is drawn by air line (23) Enter reactor, carry out catalyst regeneration, 580~740 DEG C of regeneration temperature, regenerated flue gas enters anti-by reacting product outlet (8) Product collector (10) is answered to be cooled down, subsequently into fume-dehydrating tank (19), flue gas is received from exhanst gas outlet (20) discharge Collection, waste water are discharged from wastewater outlet (18);
(3) catalyst and the analysis of raw material reactivity worth:Gaseous product that course of reaction and regenerative process are obtained, product liquid and Flue gas is analyzed, and draws the reactivity worth data of catalyst and raw material, the data are evaluated, draw catalyst and raw material Reactivity worth.
7. evaluating catalyst method as claimed in claim 6, it is characterised in that step (1) reactor operating pressure be 0.01~ 20.0MPa, reactor operation temperature are 400~680 DEG C.
8. evaluating catalyst method as claimed in claim 6, it is characterised in that step (1) reactor operating pressure be 0.1~ 15.0MPa, reactor operation temperature are 420~650 DEG C.
9. evaluating catalyst method as claimed in claim 6, it is characterised in that step (2) regenerate when char length be 1.0~ 4.0min, top absolute pressure are 0.10~0.40Mpa.
CN201711175218.0A 2017-11-22 2017-11-22 A kind of catalyst test apparatus and method Pending CN107703251A (en)

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