CN102539618A - Multi-channel high-throughput catalyst evaluation device and evaluation method - Google Patents
Multi-channel high-throughput catalyst evaluation device and evaluation method Download PDFInfo
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Abstract
The invention relates to a multi-channel high-throughput catalyst evaluation device and an evaluation method. The device comprises a feeding system, a reaction system, a cooling system, a sampling analysis system and a product collection system. Catalysts are contained in a reactor. Raw materials enter a mixing unit through a flow control unit for even mixing and enter a multi-channel reactor for reaction. After the reaction is completed, the materials are cooled and then enter a next unit, are sampled and analyzed by the sampling analysis system and enter the product collection system. Gas-liquid separation is conducted to products in a high-pressure separator. Liquid enters a product storage unit for storage. Gas is collected, emptied or correspondingly treated through a gas path. The multi-channel high-throughput catalyst evaluation device and the evaluation method are suitable for simultaneously evaluating various catalysts at the same reaction temperature and under the same reaction pressure, the catalyst screening efficiency is obviously improved, the testing time is saved and the test repeatability is good.
Description
Technical field
The invention belongs to catalyzer R&D process technical field, be specifically related to a kind of hyperchannel high-flux catalysts evaluating apparatus and evaluation method.The present invention mainly is applicable to test of the lab scale in the catalyzer R&D process or pilot plant test in the chemical processes such as petrochemical complex, pharmaceutical chemical industry and Coal Chemical Industry.
Background technology
In the chemical process such as petrochemical complex, medication chemistry and Coal Chemical Industry, the chemical reaction great majority are that the catalytic action through catalyzer realizes.Therefore, catalyzer is a kind of important catalyst in the chemical process, and can the quality of catalyzer determining a kind of production run realize, with and economy, chemical process is played crucial effects.
A kind of Study of Catalyst performance history generally will be passed through lab scale test, pilot plant test, and the application stage is amplified in industry then.Wherein, the lab scale experimental stage need be passed through a large amount of screenings and contrast test repeatedly, selects work such as appropriate catalyst active component, active component content and different mode of loading and roasting condition.In the pilot plant test stage, amplify and investigate the catalyzer that optimizes under the lab scale test condition, need a large amount of contrast tests equally.Therefore, improve the confidence level of catalyst screening efficient and contrast test, help improving the efficiency of research and development of catalyzer, shorten the construction cycle of catalyzer.
The characteristics of combinatorial chemistry are can synthesize hundreds and thousands of kinds at short notice to have the different samples of forming, and desirable chemical property is measured simultaneously, and reaction conditions is carried out rapid Optimum.The success or failure of the combinatorial chemistry of catalytic field research at present mainly are the quality of reactive system design.
The traditional screening method of catalyzer is method of trial and error, and workload is big, and efficient is not high.At present, scientists in all sorts of ways the design and set up catalyst libraries, catalyzer is carried out rapid screening, obtained many achievements.U.S. Purdue university develops a kind of automatic preparation and detects the system of zeolite molecular sieve; Each style plate has 8～19 reaction chambers (150～300 microlitre); Can test six blocks of plates simultaneously at every turn; Product reclaims with centrifugal method, and the combinatorial libraries that forms at last screens with X-ray scattering technology for detection or with electron microscope, only consumes seldom reagent and just obtains a lot of data.Because catalytic reaction is themopositive reaction, activated catalyzer can infrared one-tenth phase.Steven J.Taylor and James P.Morken utilize the infra-red heat spectrometer that the polymeric beads that is loaded with more than 3000 potential catalyst storehouse is screened, and find out the effective catalyst of two active organic compounds as the nucleophilic acidylate.
CN 1803271A discloses a kind of general shunt and high-throughout parallel catalytic reaction unit, is suitable for the fluid-solid heterogeneous catalytic reaction.This unit comprises shunt (can independently use), flow controller, parallel reaction device, temperature controller, refrigeratory and product collector.Reacting fluid gets into the total flow of a kind of fluid of control in the flow controller; Shunt through shunt then; Mix respectively with the fluid that comes out from other shunt again and obtain the multi-path fluid potpourri identical with each single shunt port number; The respective channel that gets into reactor then respectively contacts with catalyzer (each passage is adorned a kind of catalyzer), carries out catalytic reaction, thus the performance of evaluate catalysts.
CN 1830537A relates to a kind of vapor phase method synthesizing methanol that is suitable for, dimethyl ether, and the multichannel fixed bed reacter and the reaction method of the high flux screening of chemicals catalyzer such as dimethyl carbonate belong to chemical machinery field.This reactor is made up of sampling system, parallel reactor, oil bath heating unit and product acquisition system four parts.
Prior art mainly is the mode that single heating furnace and single reactor match, and ubiquity evaluating catalyst workload is big, the cycle is long and the test condition of contrast test can't guarantee that consistance, relative error problem such as can't avoid.Along with the progressively development of combinatorial chemistry to catalytic field, the aggregate velocity of catalyst libraries is more and more faster, and estimating these catalyst performances needs high-throughout instrument and method, requires the development of high flux screening technology.The mode that the present invention adopts single heating furnace and multiple reactor to match; Can estimate a plurality of identical or different catalyzer simultaneously; Improve the efficient of catalyst screening significantly, especially, under identical temperature of reaction and reaction pressure, screened catalyzer; The relative error of test condition when having eliminated contrast test has improved the confidence level of contrast test widely.The influence of temperature studies temperature of reaction that also can be through differential responses system heating furnace is set.
Summary of the invention
The present invention is directed to a series of problems that existing catalyst screening technology exists, proposed a kind of temperature control, control stream of being easy to, good airproof performance, easy and simple to handle, efficient is high, the hyperchannel high-flux catalysts evaluating apparatus and the evaluation method of safety economy.
In order to achieve the above object, the present invention realizes through following technical scheme:
The present invention at first provides a kind of hyperchannel high-flux catalysts evaluating apparatus, comprises feed system, reactive system, sample analysis system and product collection system.Said feed system comprises feeding-passage, flow controlling unit and mixed cell.Reactive system is made up of multi-channel reaction device and multi-channel reaction device external heated unit.Product collection system comprises HP separator and product storage element.More than design can realize fundamental purpose of the present invention.Below be of the present invention preferred and unrestricted about the detailed design of each parts of evaluating apparatus of the present invention, other forms that those skilled in the art can be known all can be used for embodiment of the present invention.
Between reactive system according to the invention and the sampling system cooling system can be set, cooling system is not necessary design of the present invention.The effect of cooling system is to make reaction product adjust to the temperature that is fit to sampling and measuring.If reaction product can satisfy the sampling needs through the temperature that connecting pipe arrives sampling system, can save cooling system here.Whether the setting that those skilled in the art can confirm cooling system according to actual conditions and the experience of oneself and confirms the formation of cooling system according to concrete technological requirement, to reach corresponding testing requirements.Heat interchanger for example, heat interchanger is with the equipment of the part heat transferred cold fluid of hot fluid, claims heat exchanger again.Heat interchanger is the common apparatus of chemical industry, oil, power, food and other many industrial sectors, occupies critical role aborning.Heat interchanger can be used as well heater, refrigeratory, condenser, evaporator and reboiler etc. in Chemical Manufacture, uses more extensive.Among the present invention heat interchanger is used as refrigeratory.
Multi-channel reaction device according to the invention is made up of at least two by-reaction devices, to realize the hyperchannel effect.
When feed system is set to one, between feed system and reactive system, shunt is set, each passage of shunt is corresponding one by one with each by-reaction device of multi-channel reaction device.Through shunt reaction raw materials is branched to each by-reaction device, can obtain the flow of each passage homogeneous, also can split into different flow arbitrarily according to actual needs.
When feed system was set to two or more, as not establishing shunt, then feed system was corresponding one by one with each by-reaction device of multi-channel reaction device, and the corresponding by-reaction device of feed system has been avoided the branch flow problem after the charging.If shunt is set, can require the number of feed system corresponding with the by-reaction device, make corresponding one by one the getting final product of each by-reaction device of each passage of shunt and multi-channel reaction device, increased the dirigibility of device design.
In addition, a plurality of identical by-reaction devices are heated in same heating furnace, guarantee that each by-reaction device of same reactive system possesses identical temperature of reaction.When needs assessment differential responses temperature factor, can regulate different temperature and realize through a plurality of reactive systems are set.
Feeding-passage according to the invention is the gas-phase feed passage, and flow controlling unit is a mass flow controller, is used for control, adjustments of gas inlet amount.Mass flow controller is to be used for the mass rate of all gases is carried out a kind of instrument of precision measurement and control, is used for electronic technology equipment in a large number, like diffusion; Oxidation, extension, CVD; Plasma etchings etc., and filming equipment are in the light transmitting fiber manufacturing equipment; And be widely used in industries such as petrochemical complex, metallurgy, pharmacy.The gas-phase feed passage can design according to the class number of institute's air inlet body, and corresponding mass flow controller is design respectively also, the corresponding mass flow controller of a kind of gas.For example, get into two kinds of gas H from the gas-phase feed passage
2And C
2H
4, mass flow controller is designed to H respectively so
2Mass flow controller and C
2H
4Mass flow controller.
The above feeding-passage can also comprise the liquid phase feeding passage.Quality of connection flow controller or volume pump under the demanding condition of explosive-proof grade, are preferably selected security higher quality flow controller as flow controlling unit for use behind the said liquid phase feeding passage.Volume pump is also claimed fixed displacement pump or proportioning pump, be a kind ofly can satisfy various strict process requirementss of process, flow can be in the 0.001-100% scope step-less adjustment, be used for carrying a kind of special volumetric pump of liquid (particularly corrosive liquids).If there is not liquid phase feeding in the technological requirement, need not design the liquid phase feeding passage.Those skilled in the art can carry out the selection of feeding-passage and flow controlling unit according to actual tests requirement and general knowledge, are preferred and unrestricted here.Likewise, liquid phase feeding passage, flow controlling unit also can be provided with one or more according to the actual tests situation, repeat no more at this.
Acting as of mixed cell according to the invention mixes thing mutually.When having liquid phase feed in the charging, can be at mixed cell outer setting well heater, the technician can be heated to relevant temperature according to concrete technological requirement, and liquid phase is gasified totally, and thing is mixed mutually.When even charging all is phase feed, well heater also can make the mixing of gas even more, rapid.Well heater according to the invention is selected from hotline heater, electric furnace or heat tape.Hotline heater is to be fuel with coal, heavy oil, light oil, other combustible materials of inflammable gas, and conduction oil is a thermal barrier, utilizes circulating oil pump to force the liquid phase circulation, and heat energy is flowed to behind the hot equipment, returns the single flow special type industrial furnace that reheats then.Hotline heater has low pressure, high temperature, safe, energy-efficient characteristics, has complete operation control and safety monitoring unit simultaneously, and critically Control work is quick-fried, and explosive-proof grade can reach the C level.Other unit that can be used for mixed cell, reactor external heating that those skilled in the art can be known all can be used for embodiment of the present invention.
Sample analysis according to the invention system is an on-line analysis system, can realize sampling and measuring at regular time and quantity, with influence factors such as evaluate catalysts kind, reaction time.Those skilled in the art can carry out the design and the use of sample analysis system according to actual conditions, can realize that the sampling system of online sample analysis function all can be used for the present invention.
Product collection system according to the invention comprises HP separator and product storage element.HP separator is one of major equipment in the Chemical Manufacture technique unit.When being used for technique for applying of the present invention, HP separator can guarantee that system pressure is consistent, helps keeping system stability.
The present invention also provides a kind of hyperchannel high-flux catalysts evaluation method, and catalyzer is packed in the reactor, and raw material gets in the mixed cell through flow controlling unit and mixes, and gets in the multi-channel reaction device and reacts; After reaction was accomplished, material was gone into next unit through supercooling is laggard, carries out sample analysis through the sample analysis system, and material is to product collection system simultaneously; Product carries out gas-liquid separation in HP separator, liquid phase gets in the product storage element and stores, and gas phase is collected or relevant treatment such as emptying through gas circuit.
The catalyzer that each by-reaction device is put into can be identical also can be different, sampling mode (sample time, sampling amount etc.) also can be realized through control sample analysis system, select to get final product according to the actual experiment demand.
Compare with the prior art scheme, the present invention has following beneficial effect:
1, integral body of the present invention is easy to temperature control, control stream, good airproof performance, and easy and simple to handle, efficient is high, safety economy, favorable reproducibility, flexible design according to actual needs.
2, can estimate a plurality of identical or different catalyzer simultaneously; Obviously improve the efficient of catalyst screening; Especially, under identical temperature of reaction and reaction pressure, screen catalyzer, the relative error of test condition when having eliminated contrast test; Improved the confidence level of contrast test widely, realized high flux screening a large amount of catalyzer.
3, the present invention can be used for estimating influence factors such as different catalyst active component, active component content and mode of loading, reaction time, roasting condition fast, helps improving the assess effectiveness of catalyzer.
Description of drawings
Accompanying drawing 1 is the evaluating apparatus structural representation of the specific embodiment of the invention one;
Accompanying drawing 2 is the evaluating apparatus structural representation of the specific embodiment of the invention two;
Accompanying drawing 3 is the evaluating apparatus structural representation of the specific embodiment of the invention three;
Accompanying drawing 4 is the evaluating apparatus structural representation of the specific embodiment of the invention four;
Accompanying drawing 5 is the evaluating apparatus structural representation of the specific embodiment of the invention five.
Among the figure: the 1-feed system; The 2-reactive system; 3-sample analysis system; The 4-product collection system; 5-gas-phase feed passage; The 6-mass flow controller; The 7-mixed cell; 8-multi-channel reaction device; The 9-heating unit; The 10-HP separator; 11-product storage element; The 12-heat interchanger; 13-liquid phase feeding passage; The 14-volume pump; The 15-well heater; The 16-shunt.
Down in the face of further explain of the present invention.But following instance only is a simple and easy example of the present invention, does not represent or limits rights protection scope of the present invention, and interest field of the present invention is as the criterion with claims.
Embodiment
For the present invention is described better, be convenient to understand technical scheme of the present invention, typical case of the present invention but non-restrictive example is following:
Embodiment one
A kind of hyperchannel high-flux catalysts evaluating apparatus comprises the feed system 1, reactive system 2, sample analysis system 3 and the product collection system 4 that connect successively; Said feed system 1 is two, comprises gas-phase feed passage 5, mass flow controller 6 and mixed cell 7 respectively; Reactive system 2 is made up of multi-channel reaction device 8 and multi-channel reaction device 8 external heated unit 9, and multi-channel reaction device 8 has two by-reaction devices, and feed system 1 is corresponding one by one with each by-reaction device of multi-channel reaction device 8; Product collection system is 4 for comprising HP separator 10 and product storage element 11.
Catalyzer to be evaluated is packed in each by-reaction device; Make response sample A, B pass through A mass flow controller, B mass flow controller respectively, get into simultaneously two kinds of gases are mixed, get in the multi-channel reaction device and react; After reaction was accomplished, material got into the sample analysis system and carries out sample analysis, and material is to product collection system simultaneously; Product carries out gas-liquid separation in HP separator, liquid phase gets in the product storage element and stores, and gas phase is collected or relevant treatment such as emptying through gas circuit.
Embodiment two
A kind of hyperchannel high-flux catalysts evaluating apparatus comprises the feed system 1, reactive system 2, heat interchanger 12, sample analysis system 3 and the product collection system 4 that connect successively; Said feed system 1 is four, comprises gas-phase feed passage 5 and mass flow controller 6, liquid phase feeding passage 13 and volume pump 14 and mixed cell 7 respectively, and mixed cell 7 outsides are provided with well heater 15; Reactive system 2 is two, is made up of multi-channel reaction device 8 and multi-channel reaction device external heated unit 9 respectively, and hyperchannel well heater 8 has two by-reaction devices, and feed system 1 is corresponding one by one with each by-reaction device of multi-channel reaction device 8; Product collection system 4 is two, comprises HP separator 10 and product storage element 11.
Catalyzer to be evaluated is packed in each by-reaction device; Make response sample A, B pass through A mass flow controller, B volume pump respectively, get into simultaneously two kinds of materials are mixed, get in the multi-channel reaction device and react; After reaction was accomplished, material got into the sample analysis system and carries out sample analysis after supercooling, and material is to product collection system simultaneously; Product carries out gas-liquid separation in HP separator, liquid phase gets in the product storage element and stores, and gas phase is carried out collection and treatment through gas circuit.
Embodiment three
A kind of hyperchannel high-flux catalysts evaluating apparatus comprises the feed system 1, reactive system 2, heat interchanger 12, sample analysis system 3 and the product collection system 4 that connect successively; Said feed system 1 is five, comprises gas-phase feed passage 5 and mass flow controller 6, liquid phase feeding passage 13 and mass flow controller 6 and mixed cell 7 respectively, and mixed cell 7 outsides are provided with well heater 15; Reactive system 2 is made up of multi-channel reaction device 8 and multi-channel reaction device 8 external heated unit 9, and multi-channel reaction device 8 has five by-reaction devices, and feed system 1 is corresponding one by one with each by-reaction device of multi-channel reaction device 8; Product collection system 4 is one, comprises HP separator 10 and product storage element 11.
Catalyzer to be evaluated is packed in each by-reaction device; Make response sample A, B pass through A mass flow controller, B mass flow controller respectively, get into simultaneously two kinds of materials are mixed, mix the back and get in the multi-channel reaction device and reacts; After reaction was accomplished, material got into the sample analysis system and carries out sample analysis after supercooling, and material is to product collection system simultaneously; Product carries out gas-liquid separation in HP separator, liquid phase gets in the product storage element and stores, and gas phase is collected or relevant treatment such as emptying through gas circuit.
Embodiment four
A kind of hyperchannel high-flux catalysts evaluating apparatus comprises the feed system 1, reactive system 2, heat interchanger 12, sample analysis system 3 and the product collection system 4 that connect successively; Said feed system 1 is two, comprises three gas-phase feed passages 5 and mass flow controller 6, liquid phase feeding passage 13 and a volume pump 14 and a mixed cell 7 respectively, and mixed cell 7 outsides are provided with well heater 15; Reactive system 2 is made up of multi-channel reaction device 8 and multi-channel reaction device 8 external heated unit 9, and multi-channel reaction device 8 has two by-reaction devices, and feed system 1 is corresponding one by one with two by-reaction devices of multi-channel reaction device 8; Product collection system 4 is one, comprises HP separator 10 and product storage element 11.
Catalyzer to be evaluated is packed in each by-reaction device; Make response sample A, B, C, D pass through A mass flow controller, B mass flow controller, C mass flow controller, D volume pump respectively, get into simultaneously four kinds of materials are mixed, mix the back and get in the multi-channel reaction device and reacts; After reaction was accomplished, material got into the sample analysis system and carries out sample analysis after supercooling, and material is to product collection system simultaneously; Product carries out gas-liquid separation in HP separator, liquid phase gets in the product storage element and stores, and gas phase is collected or relevant treatment such as emptying through gas circuit.
Embodiment five
A kind of hyperchannel high-flux catalysts evaluating apparatus comprises the feed system 1, reactive system 2, heat interchanger 12, sample analysis system 3 and the product collection system 4 that connect successively; Said feed system 1 comprises a gas-phase feed passage 5 and mass flow controller 6, liquid phase feeding passage 13 and a volume pump 14 and a mixed cell 7, and mixed cell 7 outsides are provided with well heater 15; Reactive system 2 is made up of multi-channel reaction device 8 and multi-channel reaction device external heated unit 9, and hyperchannel well heater 8 has four by-reaction devices; Be connected with shunt 16 behind the feed system 1, will mix the back material and be divided into four, four passages of shunt 16 are corresponding one by one with four by-reaction devices of multi-channel reaction device 8; Product collection system 4 comprises HP separator 10 and product storage element 11.
Catalyzer to be evaluated is packed in each by-reaction device; Make response sample A, B, C, D pass through A mass flow controller, B volume pump, C mass flow controller, D volume pump respectively, get into simultaneously four kinds of materials are mixed, after the shunt shunting, get in the multi-channel reaction device and react; After reaction was accomplished, material got into the sample analysis system and carries out sample analysis after supercooling, and material is to product collection system simultaneously; Product carries out gas-liquid separation in HP separator, liquid phase gets in the product storage element and stores, and gas phase is carried out collection and treatment through gas circuit.
Applicant's statement; The present invention explains detailed structure characteristic of the present invention and evaluation method through the foregoing description; But the present invention is not limited to above-mentioned detailed structure characteristic and evaluation method, does not mean that promptly the present invention must rely on above-mentioned detailed structure characteristic and evaluation method could be implemented.The person of ordinary skill in the field should understand, and to any improvement of the present invention, to the increase of the equivalence replacement of parts that the present invention selects for use and accessory, the selection of concrete mode etc., all drops within protection scope of the present invention and the open scope.
Claims (10)
1. a hyperchannel high-flux catalysts evaluating apparatus is characterized in that, comprises feed system (1), reactive system (2), sample analysis system (3) and product collection system (4); Said feed system (1) comprises feeding-passage, flow controlling unit and mixed cell (7); Reactive system (2) is made up of multi-channel reaction device (8) and multi-channel reaction device (8) external heated unit (9); Product collection system (4) comprises HP separator (10) and product storage element (11).
2. device as claimed in claim 1 is characterized in that, is provided with cooling system between said reactive system (2) and the sample analysis system (3); Said multi-channel reaction device (8) is made up of at least two by-reaction devices.
3. according to claim 1 or claim 2 device is characterized in that, between feed system (1) and the reactive system (2) shunt (16) is housed.
4. device as claimed in claim 3 is characterized in that, said feed system (1) is one; Each passage of shunt (16) is corresponding one by one with each by-reaction device of multi-channel reaction device (8).
5. like the described device of one of claim 1-3, it is characterized in that said feed system (1) is two or more; Feed system (1) or each passage of shunt (16) are corresponding one by one with each by-reaction device of multi-channel reaction device (8).
6. like the described device of one of claim 1-5, it is characterized in that said feeding-passage is gas-phase feed passage (5), flow controlling unit is mass flow controller (6).
7. device as claimed in claim 6 is characterized in that, said feeding-passage also comprises liquid phase feeding passage (13); Said liquid phase feeding passage (13) back quality of connection flow controller (6) or volume pump (14) are as flow controlling unit.
8. like the described device of one of claim 1-7, it is characterized in that said mixed cell (7) outer setting well heater (15); Said well heater (15) is selected from hotline heater, electric furnace or heat tape.
9. like the described device of one of claim 1-8, it is characterized in that said sample analysis system (3) is online sampling system, can realize taking a sample at regular time and quantity.
10. a hyperchannel high-flux catalysts evaluation method is characterized in that, catalyzer is packed in the reactor, and raw material gets in the mixed cell (7) through flow controlling unit and mixes, and gets in the multi-channel reaction device (8) and reacts; After reaction was accomplished, material was gone into next unit through supercooling is laggard, carries out sample analysis through sample analysis system (3), simultaneously material to product collection system (4); Product carries out gas-liquid separation in HP separator (10), liquid phase gets in the product storage element (11) and stores, and gas phase is collected or the emptying processing through gas circuit.
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| CN106770891A (en) * | 2016-12-30 | 2017-05-31 | 神华集团有限责任公司 | Catalyst test apparatus and evaluation method |
| CN106841447A (en) * | 2017-02-15 | 2017-06-13 | 中国工程物理研究院材料研究所 | A kind of VPCE static properties method of testing |
| US11344860B2 (en) | 2019-09-30 | 2022-05-31 | Saudi Arabian Oil Company | Multiple reactor system for parallel catalyst testing |
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| CN102539618B (en) | 2015-02-25 |
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