CN202410622U - Multi-channel high-flux catalyst evaluation device - Google Patents
Multi-channel high-flux catalyst evaluation device Download PDFInfo
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- CN202410622U CN202410622U CN2012200082898U CN201220008289U CN202410622U CN 202410622 U CN202410622 U CN 202410622U CN 2012200082898 U CN2012200082898 U CN 2012200082898U CN 201220008289 U CN201220008289 U CN 201220008289U CN 202410622 U CN202410622 U CN 202410622U
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Abstract
The utility model relates to a multi-channel high-flux catalyst evaluation method and an evaluation device. The evaluation device comprises a feeding system, a reaction system, a cooling system, a sampling analysis system and a product collecting system. Catalysts are placed into a reactor, raw materials enter a mixing unit through a flow control unit, are uniformly mixed and enter a multi-channel reactor for reaction, and the materials enter a next unit after reaction and cooling, are sampled and analyzed by the sampling analysis system, and enter the product collecting system. Gas and liquid of products are separated in a high-pressure separator, the liquid enters a product storage unit and is stored, and the gas is collected by a gas path or correspondingly treated by means of emptying and the like. The evaluation device is applicable to simultaneously evaluating various catalysts at the same reaction temperature and under the same reaction pressure, catalyst screening efficiency is obviously improved, testing time is saved, and testing repeatability is high.
Description
Technical field
The utility model belongs to catalyst R&D process technical field, is specifically related to a kind of multichannel high-flux catalysts evaluating apparatus.The utility model mainly is applicable to test of the lab scale in the catalyst R&D process or pilot plant test in the chemical processes such as petrochemical industry, pharmaceutical chemical industry and Coal Chemical Industry.
Background technology
In the chemical process such as petrochemical industry, medication chemistry and Coal Chemical Industry, the chemical reaction great majority are that the catalytic action through catalyst realizes.Therefore, catalyst is a kind of important catalyst in the chemical process, and can the quality of catalyst determining a kind of production process realize, with and economy, chemical process is played crucial effects.
A kind of Study of Catalyst development process 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 catalyst that optimizes under the lab scale experimental 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 catalyst, shorten the construction cycle of catalyst.
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 condition is carried out rapid Optimum.The success or failure of the combinatorial chemistry of catalytic field research at present mainly are the quality of reaction system design.
The traditional screening method of catalyst is trial and error procedure, and workload is big, and efficient is not high.At present, scientists in all sorts of ways the design and set up catalyst libraries, catalyst 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 reative cells (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 exothermic reaction, activated catalyst 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 current divider and high-throughout parallel catalytic reaction unit, is suitable for the fluid-solid heterogeneous catalytic reaction.This unit comprises current divider (can independently use), flow controller, parallel reaction device, temperature controller, cooler and product collector.Reacting fluid gets into the total flow of a kind of fluid of control in the flow controller; Shunt through current divider then; Mix respectively with the fluid that comes out from other current divider again and obtain the multi-path fluid mixture identical with each single current divider port number; The respective channel that gets into reactor then respectively contacts with catalyst (each passage is adorned a kind of catalyst), 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 catalyst 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 experimental condition of contrast test can't guarantee that uniformity, 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 utility model adopts single heating furnace and multiple reactor to match; Can estimate a plurality of identical or different catalyst simultaneously; Improve the efficient of catalyst screening significantly, especially, under identical reaction temperature and reaction pressure, screened catalyst; The relative error of experimental condition when having eliminated contrast test has improved the confidence level of contrast test widely.The influence of temperature studies reaction temperature that also can be through differential responses system heating furnace is set.
The utility model content
The utility model has proposed a kind of temperature control, control stream of being easy to a series of problems that existing catalyst screening technology exists, good airproof performance, and easy and simple to handle, efficient is high, the multichannel high-flux catalysts evaluating apparatus of safety economy.
In order to achieve the above object, the utility model is realized through following technical scheme:
The utility model at first provides a kind of multichannel high-flux catalysts evaluating apparatus, comprises feed system, reaction system, sample analysis system and product collection system.Said feed system comprises feeding-passage, flow controlling unit and mixed cell.Reaction system is made up of multi-channel reaction device and multi-channel reaction device external heated unit.Product collection system comprises high-pressure separator and product storage element.More than design can realize the main purpose of the utility model.Below be the preferred and unrestricted of the utility model about the detailed design of each parts of the utility model evaluating apparatus, other forms that those skilled in the art can be known all can be used for implementing the utility model.
Between said reaction system of the utility model and the sampler cooling system can be set, cooling system is not necessity design of the utility model.The effect of cooling system is to make product adjust to the temperature that is fit to sampling and measuring.If product can satisfy the sampling needs through the temperature that tube connector arrives sampler, 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 test requirements document.Heat exchanger for example, heat exchanger is with the equipment of the part heat transferred cold fluid of hot fluid, claims heat exchanger again.Heat exchanger is the common apparatus of chemical industry, oil, power, food and other many industrial departments, occupies critical role aborning.Heat exchanger can be used as heater, cooler, condenser, evaporimeter and reboiler etc. in Chemical Manufacture, uses more extensive.In the utility model heat exchanger is used as cooler.
The said multi-channel reaction device of the utility model is made up of at least two by-reaction devices, to realize the multichannel effect.
When feed system is set to one, between feed system and reaction system, current divider is set, each passage of current divider is corresponding one by one with each by-reaction device of multi-channel reaction device.Through current divider 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 current divider, 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 current divider 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 current divider and multi-channel reaction device, increased the flexibility 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 reaction system possesses identical reaction temperature.When needs assessment differential responses temperature factor, can regulate different temperature and realize through a plurality of reaction systems are set.
The said feeding-passage of the utility model 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 flow of all gases is carried out a kind of instrument of accurate 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 optical fiber manufacturing equipment; And be widely used in industries such as petrochemical industry, 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 measuring 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.Measuring pump is also claimed constant 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 displacement 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 the said mixed cell of the utility model mixes thing mutually.When having liquid phase feed in the charging, can be at mixed cell outer setting heater, the technical staff 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, heater also can make the mixing of gas even more, rapid.The said heater of the utility model 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 fuel gas, and conduction oil is a heat carrier, utilizes oil circulating 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 it is quick-fried critically to control work, and explosive-proof grade can reach the C level.Other unit that can be used for mixed cell, reactor external heat that those skilled in the art can be known all can be used for implementing the utility model.
The said sample analysis of the utility model 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 sampler of online sample analysis function all can be used for the utility model.
The said product gathering system of the utility model comprises high-pressure separator and product storage element.High-pressure separator is one of capital equipment in the Chemical Manufacture technique unit.When being used for the utility model technique for applying, high-pressure separator can guarantee that system pressure is consistent, helps keeping system stability.
The utility model also provides a kind of multichannel high-flux catalysts evaluation method, and catalyst 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 high-pressure 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 catalyst 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 utlity model has following beneficial effect:
1, the utility model integral body 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 catalyst simultaneously; Obviously improve the efficient of catalyst screening; Especially, under identical reaction temperature and reaction pressure, screen catalyst, the relative error of experimental condition when having eliminated contrast test; Improved the confidence level of contrast test widely, realized high flux screening a large amount of catalyst.
3, the utility model 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 catalyst.
Description of drawings
Accompanying drawing 1 is the evaluating apparatus structural representation of the utility model specific embodiment one;
Accompanying drawing 2 is the evaluating apparatus structural representation of the utility model specific embodiment two;
Accompanying drawing 3 is the evaluating apparatus structural representation of the utility model specific embodiment three;
Accompanying drawing 4 is the evaluating apparatus structural representation of the utility model specific embodiment four;
Accompanying drawing 5 is the evaluating apparatus structural representation of the utility model specific embodiment five.
Among the figure: the 1-feed system; The 2-reaction 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-high-pressure separator; 11-product storage element; The 12-heat exchanger; 13-liquid phase feeding passage; The 14-measuring pump; The 15-heater; The 16-current divider.
Down in the face of the utility model further explain.But following instance only is the simple and easy example of the utility model, does not represent or limit the rights protection scope of the utility model, and the interest field of the utility model is as the criterion with claims.
The specific embodiment
For the utility model is described better, be convenient to understand the technical scheme of the utility model, the typical case of the utility model but non-restrictive example is following:
Embodiment one
A kind of multichannel high-flux catalysts evaluating apparatus comprises the feed system 1, reaction 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; Reaction 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 high-pressure separator 10 and product storage element 11.
Catalyst 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 high-pressure 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 multichannel high-flux catalysts evaluating apparatus comprises the feed system 1, reaction system 2, heat exchanger 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 measuring pump 14 and mixed cell 7 respectively, and mixed cell 7 outsides are provided with heater 15; Reaction system 2 is two, is made up of multi-channel reaction device 8 and multi-channel reaction device external heated unit 9 respectively, and multichannel 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 high-pressure separator 10 and product storage element 11.
Catalyst to be evaluated is packed in each by-reaction device; Make response sample A, B pass through A mass flow controller, B measuring 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 high-pressure 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 multichannel high-flux catalysts evaluating apparatus comprises the feed system 1, reaction system 2, heat exchanger 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 heater 15; Reaction 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 high-pressure separator 10 and product storage element 11.
Catalyst 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 high-pressure 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 multichannel high-flux catalysts evaluating apparatus comprises the feed system 1, reaction system 2, heat exchanger 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 measuring pump 14 and a mixed cell 7 respectively, and mixed cell 7 outsides are provided with heater 15; Reaction 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 high-pressure separator 10 and product storage element 11.
Catalyst 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 measuring 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 high-pressure 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 multichannel high-flux catalysts evaluating apparatus comprises the feed system 1, reaction system 2, heat exchanger 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 measuring pump 14 and a mixed cell 7, and mixed cell 7 outsides are provided with heater 15; Reaction system 2 is made up of multi-channel reaction device 8 and multi-channel reaction device external heated unit 9, and multichannel heater 8 has four by-reaction devices; Be connected with current divider 16 behind the feed system 1, will mix the back material and be divided into four, four passages of current divider 16 are corresponding one by one with four by-reaction devices of multi-channel reaction device 8; Product collection system 4 comprises high-pressure separator 10 and product storage element 11.
Catalyst to be evaluated is packed in each by-reaction device; Make response sample A, B, C, D pass through A mass flow controller, B measuring pump, C mass flow controller, D measuring pump respectively, get into simultaneously four kinds of materials are mixed, after the current divider 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 high-pressure 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 utility model is explained the detailed structure characteristic and the evaluation method of the utility model through the foregoing description; But the utility model is not limited to above-mentioned detailed structure characteristic and evaluation method, does not mean that promptly the utility model must rely on above-mentioned detailed structure characteristic and evaluation method could be implemented.The person of ordinary skill in the field should understand; Any improvement to the utility model; To the increase of the equivalence replacement of parts that the utility model is selected for use and accessory, the selection of concrete mode etc., within the protection domain that all drops on the utility model and the open scope.
Claims (9)
1. a multichannel high-flux catalysts evaluating apparatus is characterized in that, comprises feed system (1), reaction 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); Reaction 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 high-pressure 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 reaction 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 reaction system (2) current divider (16) is housed.
4. device as claimed in claim 3 is characterized in that, said feed system (1) is one; Each passage of current divider (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 current divider (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 measuring 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 heater (15); Said 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 sampler, can realize taking a sample at regular time and quantity.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012200082898U CN202410622U (en) | 2012-01-10 | 2012-01-10 | Multi-channel high-flux catalyst evaluation device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012200082898U CN202410622U (en) | 2012-01-10 | 2012-01-10 | Multi-channel high-flux catalyst evaluation device |
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| CN202410622U true CN202410622U (en) | 2012-09-05 |
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| CN2012200082898U Expired - Fee Related CN202410622U (en) | 2012-01-10 | 2012-01-10 | Multi-channel high-flux catalyst evaluation device |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102539618A (en) * | 2012-01-10 | 2012-07-04 | 北京昊诚油气科技有限公司 | Multi-channel high-throughput catalyst evaluation device and evaluation method |
| CN108745212A (en) * | 2018-06-27 | 2018-11-06 | 安徽科幂机械科技有限公司 | A kind of desktop grade fixed bed of successive reaction |
-
2012
- 2012-01-10 CN CN2012200082898U patent/CN202410622U/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102539618A (en) * | 2012-01-10 | 2012-07-04 | 北京昊诚油气科技有限公司 | Multi-channel high-throughput catalyst evaluation device and evaluation method |
| CN102539618B (en) * | 2012-01-10 | 2015-02-25 | 北京昊诚油气科技有限公司 | Multi-channel high-throughput catalyst evaluation device and evaluation method |
| CN108745212A (en) * | 2018-06-27 | 2018-11-06 | 安徽科幂机械科技有限公司 | A kind of desktop grade fixed bed of successive reaction |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20120905 Termination date: 20180110 |
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| CF01 | Termination of patent right due to non-payment of annual fee |