CN108267346A - The high-throughput preparation system and method for sieve sample - Google Patents
The high-throughput preparation system and method for sieve sample Download PDFInfo
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- CN108267346A CN108267346A CN201611269955.2A CN201611269955A CN108267346A CN 108267346 A CN108267346 A CN 108267346A CN 201611269955 A CN201611269955 A CN 201611269955A CN 108267346 A CN108267346 A CN 108267346A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 50
- 238000002425 crystallisation Methods 0.000 claims abstract description 31
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 26
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 26
- 230000008025 crystallization Effects 0.000 claims abstract description 19
- 239000002994 raw material Substances 0.000 claims abstract description 16
- 238000000926 separation method Methods 0.000 claims abstract description 4
- 239000002808 molecular sieve Substances 0.000 claims description 28
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 28
- 238000012216 screening Methods 0.000 claims description 22
- 238000004458 analytical method Methods 0.000 claims description 19
- 238000004140 cleaning Methods 0.000 claims description 16
- 238000002474 experimental method Methods 0.000 claims description 14
- 238000001914 filtration Methods 0.000 claims description 14
- 238000012545 processing Methods 0.000 claims description 13
- 238000000634 powder X-ray diffraction Methods 0.000 claims description 12
- 239000002904 solvent Substances 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 11
- 238000013461 design Methods 0.000 claims description 8
- 238000001514 detection method Methods 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 8
- 238000011160 research Methods 0.000 claims description 7
- 238000011161 development Methods 0.000 claims description 5
- 238000007405 data analysis Methods 0.000 claims description 4
- 230000033001 locomotion Effects 0.000 claims description 4
- 238000002441 X-ray diffraction Methods 0.000 claims description 3
- 230000008859 change Effects 0.000 claims description 3
- 238000005070 sampling Methods 0.000 claims description 3
- 230000032683 aging Effects 0.000 abstract description 8
- 230000008569 process Effects 0.000 description 14
- 239000000463 material Substances 0.000 description 10
- 229910021536 Zeolite Inorganic materials 0.000 description 8
- 238000010586 diagram Methods 0.000 description 8
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- 239000010457 zeolite Substances 0.000 description 8
- 238000001035 drying Methods 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 3
- 229910052593 corundum Inorganic materials 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910001845 yogo sapphire Inorganic materials 0.000 description 3
- 241001269238 Data Species 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 125000005842 heteroatom Chemical group 0.000 description 2
- 239000012452 mother liquor Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 238000010189 synthetic method Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- ILRRQNADMUWWFW-UHFFFAOYSA-K aluminium phosphate Chemical compound O1[Al]2OP1(=O)O2 ILRRQNADMUWWFW-UHFFFAOYSA-K 0.000 description 1
- 229940001007 aluminium phosphate Drugs 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 238000013528 artificial neural network Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000009514 concussion Effects 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000013178 mathematical model Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000012621 metal-organic framework Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- NJPPVKZQTLUDBO-UHFFFAOYSA-N novaluron Chemical compound C1=C(Cl)C(OC(F)(F)C(OC(F)(F)F)F)=CC=C1NC(=O)NC(=O)C1=C(F)C=CC=C1F NJPPVKZQTLUDBO-UHFFFAOYSA-N 0.000 description 1
- 238000000879 optical micrograph Methods 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000005464 sample preparation method Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 238000003828 vacuum filtration Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B37/00—Compounds having molecular sieve properties but not having base-exchange properties
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B37/00—Compounds having molecular sieve properties but not having base-exchange properties
- C01B37/06—Aluminophosphates containing other elements, e.g. metals, boron
- C01B37/08—Silicoaluminophosphates [SAPO compounds], e.g. CoSAPO
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/54—Phosphates, e.g. APO or SAPO compounds
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- Pathology (AREA)
- Immunology (AREA)
- General Physics & Mathematics (AREA)
- General Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
Present invention is disclosed a kind of synthesis of high-throughput sieve sample and detecting system and methods, it includes centralization ageing crystallization system and centrifugal separation system, wherein centralization ageing crystallization system includes the rotatable stent of one or more quantity, several retort are provided on each stent, several reaction chambers are provided in each retort, centralization ageing crystallization system provides the control separately from other retort for each retort, so that the sieve sample in several reaction chambers in each retort is synthesized at identical conditions, and the condition of each retort can be different from other retort.In use, after centralization ageing crystallization system part of the sieve sample raw material successively by system is handled, handled via centrifugal separation system part, so as to fulfill the preparation of the high-throughput sieve sample of whole system.
Description
【Technical field】
The present invention relates to the sieve sample preparation systems and method of a kind of high throughput.
【Background technology】
Molecular sieve type is various, including zeolite molecular sieve, aluminium phosphate molecular sieve, mesopore molecular sieve, metal organic framework point
Son sieve etc., their majorities are synthesized by hydro-thermal or solvent thermal process.There are many factor for influencing hydro-thermal and solvent thermal reaction, such as raw material
Type, proportioning, solvent, template, pH, temperature, time etc., the variation of these factors often influence success rate and the production of synthesis
The quality of product.
Before high throughput experimental technique is introduced into Zeolite synthesis, the synthesis and preparation of novel molecular sieve depend on
Repetition test again and again a, in this way, process costly, the period is very long is often undergone in the exploitation of new molecular sieve.
Although people also have made great progress the structure and property Quality Research of molecular sieve, still fail to develop and divide for predicting
Sub- screen banks is theoretical into, structure and performance-relevant regularity.So that in most cases, it has to by experience and intuition
It attempts to screen and find new molecular sieve.Undoubtedly, this development process inefficiency seriously restricts novel molecular sieve material
The synthesis and exploitation of material.
Fortunately, this situation is getting a new look.Help has been found in material educational circles, and they walk out this material
The method for developing predicament, that is,：High-throughput experimental technique.
High-throughput experimental technique with Zeolite synthesis be combined be Zeolite synthesis a big progress.High-throughput molecular sieve closes
Into having abandoned traditional composition rule, and instead with reliable reaction and simple and effective purification process, in same reactor
It is interior to prepare multi-products simultaneously using identical condition, then carry out the post processing of batch.
Specifically, it is assumed that given one is tested, and has silicon source 1, silicon source 1, template 1, alkali 1 in starting material
A, hetero atom 1, solvent 1, combination thereof mode is using SiO2/Al2O3Point 20 steps are completed between 1-100, and template/
Al2O3Point 20 steps are completed between 1-20, hetero atom/Al2O3Point 10 steps are completed between 0-10, and pH value range is between 7-14
10 steps is divided to complete, by calculating, such raw material and combinations thereof mode needs 101871 experiments.An if research group one
It can complete 20 experiments, be calculated by 250 days within 1 year, then he needs the time of about 20 years that could complete；And using high pass
Synthetic method is measured, if consersion unit has 384 reactors, a research group tests for one day with regard to that can complete 384, then
He only needs the time of about 1 year that can just complete.
Compared with traditional Zeolite synthesis experimental technique, the sharpest edges of high-throughput experimental technique are exactly that it allows quickly
A large amount of reaction system is systematically studied, being carried out continuously synthesis and characterization is, can rationally plan as a whole the room and time of reaction.With
Traditional synthetic method is compared, and high-throughput Zeolite synthesis method has unrivaled excellent in terms of Fast back-projection algorithm and screening
Gesture.
【Invention content】
The one side that the present invention designs is to provide a kind of workflow of the sieve sample research/development platform of high throughput,
Include design, raw material preparation, sample library preparation, sieve sample synthesis, sample analysis and the data analysis of sieve sample
Six comprising modules.Its flow chart please refers to Fig.1 shown.Concretely：
1. molecular sieve designs
Molecular sieve design module includes two large divisions：Component designs and flow scheme design.This module is mainly using design
Molecular sieve software the various combinations of selected starting material and each process parameter are set.
2. raw material prepares
Raw material preparation module mainly prepares inhomogeneous mother liquor, such as：Silicon source, silicon source, solvent, template, soda acid, miscellaneous original
Son, mineralizer, crystal seed.It may all contain one or more of mother liquors per one kind mother liquor.It is labelled, it is positioned over defined position
On.In process for preparation, agitating mode can be used, not agitating mode can also be used.
3. prepared by sample library
It is mainly what is completed by liquid distributor that sample library, which prepares module,.Combination i.e. according to set by molecular sieve software
Mode parameter moves on to each product combined in each reactor by liquid distributor.Crystal seed can be added as needed on
's.Whole process is that batch carries out, and has thus obtained the set that many products are formed, i.e. sample library.In addition, whole
During a, according to the setting of process parameter, temperature control can be used and control what the mode stirred carried out.
4. sample synthesizes
Sample synthesis module is the core of whole flow process.It mainly includes ageing (Aging), crystallization (Crystali-
Zation it) is tested with sample treatment.Temperature parameter (temperature programming, constant temperature, the program cooling needed in ageing and crystallization experiments
Deng) and mixing parametric (agitating mode and mixing speed etc.) can be set by the process parameter in molecular sieve software or
Modification.Sample treatment experiment mainly includes three steps：Washing, the transfer of dry and sample.Centrifugation can be used in washing process
Mode of washing carries out or can be used vacuum filtration mode progress；Drying mode can be used electrothermal method and carry out or can be used infrared
Line mode of heating carries out；The transfer of sample uses the branch mode of array.Above-mentioned sample washing and heating process are certainly
It is carried out in batches under conditions of dynamicization, without artificial operation.
5. sample analysis
Sample analysis module mainly include XRPD (X-ray Powder Diffraction, XRPD) test, morphology observation,
Sample roasts and yield analysis.XRPD tests are completed using the x-ray powder diffraction instrument of automation.Morphology observation is using online
What CCD (Charge Couple Device, CCD) optical microphotograph image Detection Techniques carried out.Sample roasting is using calciner
The operations such as temperature programming, constant temperature, program cooling are carried out to sample with the temperature parameter according to setting.Yield analysis is using accurate
Electronic balance measures, and measured value is output in computer and is calculated by software for calculation, and is rapidly judged by software for calculation
Its yield height.
6. data analysis
Data analysis module includes data processing, phasor making and model analysis etc..Data processing is mainly to a large amount of
Test data in effectively analyzed and screened, so as to produce it is different composition the object phase of product between two dimensions or three
The phasor of dimension or higher-dimension.The introducing of model analysis (such as neural network analysis methods), is conducive to data processing and the making of phasor,
Be conducive to the exploitation of novel molecular sieve material.
Further, another aspect of the present invention is to provide high-throughput multigroup screening technique and system, selects and meets the requirements
Sieve sample.Specifically, screening is divided into primary screener, two level screening, three level screen, until enlarged experiment link.It is whole
A screening process schematic diagram is as shown in Figure 2.The purpose of wherein primary screener is from numerous sieve sample compound experiments,
Find the structure of new sieve sample；And two level, three-level and enlarged experiment are then as a result, passing through increasing according to previous screening
Adduction is into the amount of newfound sieve sample and change synthesis condition, come the more property of new molecular sieve further obtained
It can feature.
One side of the present invention is to provide a kind of high-throughput sieve sample available for sieve sample screening
Preparation system, technical solution is：A kind of preparation system of high-throughput sieve sample available for sieve sample screening,
It includes centralized ageing-crystallization system and centrifugal separation system, wherein centralized ageing-crystallization system include it is multiple anti-
Chamber is answered, these reaction chambers are divided into or are positioned at least two reaction modules, for example, reaction vessel or cavity volume (Container)；
Any of which reaction module includes at least one or more reaction chamber, and system is provided for each reaction module independently of other moulds
The control of block so that the synthesis condition of the sieve sample of the reaction chamber of each module can be different from the molecular sieve of other modules
The synthesis condition of sample；In use, sieve sample raw material is after centralized ageing-crystallization system processing, via centrifugation
Piece-rate system processing, so as to fulfill the preparation of the high-throughput sieve sample of whole system.Further, it is wherein centralized old
Change-crystallization system includes the control of its each reaction module pressure control, temperature control, raw material are inserted/samples control, automatically
Stirring and hydrothermal/solvent thermal synthesis control etc..Further, above system is generally used for but is not limited to primary sieve sample
Screening process.
Further, in centralized ageing-crystallization system, the reaction chamber that wherein reaction module includes is can to move
So that it can carry out the static monitor of sieve sample, and can carry out the dynamic synthesis of sieve sample；It is wherein anti-
Answering the movement velocity of chamber can set, and the motion mode of reaction chamber can be people known to industry with motion mode, specifically
For, can be that several reaction chambers are set to one and can be rotated on pedestal etc..The reaction chamber that each reaction module includes
Quantity be to be set by demand, changeable, and the quantity of reaction chamber that differential responses module includes can be identical can not also
Together, with actual needs set, the quantity of reaction chamber in total at 2 or more, be specifically as follows 10,50,100,150,
200,300,500,1000 etc., but do not limit maximum quantity.Further, each reaction module may be provided with temperature
Regulating device and pressure-regulating device are spent, to realize control of the system to the independent pressure and temperature of each reaction module,
Middle temperature range can be between 0~500 degree Celsius, between room temperature~300 degree Celsius, and pressure limit is between 0~10Mpa；
The volume range of reaction chamber in reaction module between 1~100 milliliter, can be specifically 5 milliliters, 10 milliliters, 15 milliliters, 20
Milliliter, 30 milliliters, 50 milliliters, 80 milliliters etc.；The material for forming reaction chamber can be arbitrary satisfactory known to industry
Material, such as metal, nonmetallic materials, Teflon material etc..
Further, for centralized ageing ,-pressure that crystallization system provides controls, temperature controls, raw material is inserted/samples
The various functions of control, automatic stirring and hydrothermal/solvent thermal synthesis control various as known to industry can have this kind of function
Device realize.
Further, centralized ageing-crystallization system can be combined with automatic technology, real by computer system and software
The automation mechanized operation of existing whole system.Specific embodiment can be mode known to industry.
Further, it in the embodiment of a centralized ageing-crystallization system, please refers to shown in Fig. 3, wherein concentrating
Formula ageing-crystallization system 30 includes several reaction modules 31,32,33,34 individually controlled, and each reaction module includes can
The stent 310,320,330,340,350,360 of rotation, be provided on each stent several retort (for one of them,
As shown in Figure 4) 311,312,313,314,315,316, each retort 311 (as shown in Figure 5) includes main body 3111, reaction
Chamber supporter 3112, several reaction chambers 3113, reaction chamber lid 3114 and reaction cover 3115.In other alternative embodiments
In, wherein each retort can also be used as a reaction module, system provides each retort individual control, specifically
Control, automatic stirring and hydrothermal/solvent thermal synthesis control etc. are inserted/sample including pressure control, temperature control, raw material.
Further, automatic centrifugation piece-rate system can be the product of any centrifuge known to industry.Specific real
It applies in scheme, the different types of centrifuge sold in the market can be selected as needed.
Another aspect of the present invention is to provide a kind of high-throughput molecular sieve sample available for sieve sample screening
The preparation system of product, technical solution are：A kind of high throughput molecular sieve preparation system includes free-standing crystallization system and clear
Wash filtration system；Wherein free-standing crystallization system includes several reactors individually controlled, the molecular sieve in each reactor
Preparation or reaction condition of the preparation or reaction condition of sample independently of the sieve sample in other reactors；Cleaning filtering system
System can provide the function of cleaning, filtering and the drying to sample；In use, several sieve sample raw materials are first via free-standing brilliant
Change system processing forms primary sieve sample, sieve sample is formed in the processing via cleaning filtration system, so as to complete
The preparation of the high-throughput sieve sample of whole system.Further, system includes temperature to the control that each reactor provides
The control of degree and time, the control for controlling, detecting in real time for controlling, feeding in real time or sampling of independent stirring etc..Above-mentioned system
System can be used for but be not limited to the secondary screening processes of sieve sample.
Further, the quantity for the separate reactors that free-standing crystallization system includes can be adjusted specifically with the need, not had
Body limits；It is additionally provided on reactor for adjusting the temperature-adjusting device of temperature of reactor, for adjusting reactor pressure
Pressure-regulating device, in stirred reactor reaction chamber raw material mix agitating device and for detecting reactor in real time it is anti-
Answer the detection device of intracavitary situation.Wherein temperature-adjusting device, pressure-regulating device, agitating device, detection device can be industry
The known all types of device with this function on boundary；Specifically, agitating device can be agitator arm device, stirring
It can be magnetic stirring；Detection device can be acidity detector, pressure-detecting device, temperature-detecting device etc..Further
, reactor has further included raw material input/output unit, for the input and output of raw material.
Further, free-standing crystallization system can be combined with automatic technology, be realized by computer system and software whole
The automation mechanized operation of a system.Specific embodiment can be mode known to industry.
Further, it in the embodiment of a free-standing crystallization system, please refers to shown in Fig. 6, free-standing crystallization system
System 60 includes several independent reactors 61,62,63,64；Each reactor 61 (by taking a reactor as an example, please refers to Fig. 7
It is shown) include the interior main body 611 for setting reaction chamber 610, impeller stirring device 612, detection device 613, charging/sampling opening
614 and cover 615.
Further, in the embodiment for cleaning filtration system at one, a kind of cleaning filtration system includes several mistakes
Container, cleaning device and drying device are filtered, wherein filtering container is used to hold via the processed sample of free-standing crystallization system,
Cleaning device is used for each filtering container injection cleaning liquid with cleaning sample, and drying device is used for drying sample.It cleaned
Each component part in filter system can be the various devices that can realize cleaning, filtering and functions/drying known to industry；Tool
For body, cleaning device can be liquid distributor, and drying device can be concussion heating platform.
Further, high-throughput Zeolite synthesis system of the present invention can also at sample analysis system and data
Reason system is used in combination so that the synthesis and screening of sample molecule sieve can be completed once.Wherein sample analysis system can be
Arbitrary system known to industry, for example, X-ray diffraction system (X-Ray Diffraction, XRD system), X-ray powder spread out
Penetrate instrument (X-ray Powder Diffraction, XRPD).
Data processing system includes data processing, phasor and model analysis.With what is obtained via X-ray powder diffraction instrument
Data instance carries out it data processing and refers to analyze various object phases from a large amount of XRPD test datas, then, according to not
Phasor is produced with composition or the relationship between variable and not jljl phase.Wherein, object phase analysis and judgement be entire data point
The key of analysis.If singly screened to data using artificial method, this is a very arduous and numerous and diverse job.
Therefore, it is usually analyzed by the method for software.However, any one software can not also accomplish the data or diffraction from XRPD
Figure just can absolutely accurately identify the object phase of this substance.Therefore, this just need software and it is artificial between be combined.Specific place
Reason process is as follows：
First, from a large amount of XRPD test datas, classified using " grader " software to these data or spectrogram,
One kind is classified as with same or similar data or spectrogram, different data or spectrogram are classified as different types respectively.Per a kind of
Data or spectrogram all have corresponding composition or variable.
Secondly, the result of above-mentioned classification is confirmed using manual method, and by the object phase spectrogram of every one kind with marking
Quasi- spectrogram contrasts, so as to judge the object phase of all kinds of substances.If that class substance is amorphous, that class substance is target molecule
Sieve, that class substance are unknown substance, that class substance is mixture, etc..
Finally, according to above-mentioned classification as a result, depicting different compositions or variable and not jljl phase using mapping software
Between the two dimension, three-dimensional or the multidimensional phasor that are formed.
Model analysis is based on the basis of mathematical model, by modeling technique and high-throughput Zeolite synthesis experimental method knot
Altogether, the object phase of product can directly predict with the relationship of composition or variable from the model established.It can be seen that mould
Type analysis is conducive to the making improved with phasor of data, is conducive to the exploitation of novel molecular sieve material.
Relative to the preparation system of high-throughput sieve sample that the prior art, the present invention disclose, can disposably complete big
The preparation and processing of sieve sample are measured, obtains the data of a large amount of sieve sample so that industry can be according to the data of acquisition
Sieve sample is screened, filters out and meets necessarily required molecular sieve, so as to meet the research and development needs of industry.
【Description of the drawings】
Fig. 1 is the work flow diagram of the sieve sample research/development platform of high throughput of the present invention；
Fig. 2 is in the building-up process of molecular sieve of the present invention, using high-throughput techniques, carries out the flow of multistage screening
Figure；
Fig. 3 is one of the high-throughput molecular sieve preparation system of the present invention available for sieve sample primary screener
The schematic diagram of embodiment；
Fig. 4 is stent shown in Fig. 3 and the schematic diagram of the retort set thereon；
Fig. 5 is the perspective exploded view of retort shown in Fig. 4；
Fig. 6 is one of the high-throughput molecular sieve preparation system of the present invention available for the screening of sieve sample two level
The schematic diagram of embodiment；
Fig. 7 is the sectional view of reactor shown in fig. 6；
Fig. 8 is the schematic diagram of a specific embodiment of high-throughput molecular sieve preparation system of the present invention；
Fig. 9 is the schematic diagram of another specific embodiment of high-throughput molecular sieve preparation system of the present invention；
Figure 10 is the schematic diagram of a specific embodiment of one of the present invention automatic cleaning filtration system.
【Specific embodiment】
One centralized ageing-crystallization system can embodiment：
It please refers to shown in Fig. 8, a centralized ageing-crystallization system 80 includes 2 rotatable support frames 81, each
Stent tow sides are respectively arranged with 6 retort 82,16 reaction chambers of setting in each retort, in this way, system in total 384
A reaction chamber can carry out 384 groups of molecular sieve sample preparations.Further, system provides each retort temperature and controls, is automatic
Stirring and the function of hydrothermal/solvent thermal synthesis.The main performance and characteristics of the system are as follows：Operating pressure：6MPa, temperature range：
Room temperature~220 DEG C, rotating speed：It is continuously adjustable：0~50rpm.The system can be used for the primary screener of sieve sample.
One free-standing crystallization system can embodiment：
It please refers to shown in Fig. 9, a free-standing crystallization system 90 is each including 32 independently arranged reactors 91
The capacity of reactor is 200 milliliters, and the agitating device in reactor is stirred for motor driven impeller, mixing speed 1000rpm,
Detection device is pH detectors.System each reactor is provided independent temperature control, independent stirring, online pH detections, real-time sample introduction,
Hydrothermal/solvent thermal synthesis function, wherein temperature range is between room temperature~220 DEG C, pressure ＜ 6MPa.The system can be used for molecule
Sieve the two level screening of sample.
One automatic cleaning filtration system can embodiment：
Please refer to Fig.1 shown in 0, automatic cleaning filtration system 100 its include several filters 101, automatic liquid matching
System 102 and vibrations heating platform 103.Its mode of operation is to be placed in preliminary synthesis of molecular sieve sample in filter respectively,
The sample in each filter is cleaned by automatic liquid mixing system, by vibrations heating platform to the filter that sets thereon into
Row oscillation and heating.The system can be used for the two level of sieve sample to screen.
Claims (10)
1. a kind of high-throughput sieve sample preparation system available for sieve sample screening, it is characterised in that：It includes
Centralized ageing-crystallization system and centrifugal separation system, wherein centralized ageing-crystallization system includes 2 or more quantity
Reaction chamber, these reaction chambers are divided into or are positioned at least two reaction modules, and each reaction module includes at least one anti-
Chamber is answered, system provides the control independently of other reaction modules for each reaction module.
2. high throughput sieve sample preparation system as described in claim 1, it is characterised in that：Wherein centralized ageing-crystalline substance
Change system includes pressure control to the control of its each reaction module, temperature controls, control, automatic stirring are inserted/sampled to raw material
And at least one of hydrothermal/solvent thermal synthesis control etc..
3. high throughput sieve sample preparation system as described in claim 1, it is characterised in that：Wherein described reaction chamber can be with
Movement, reaction module are provided with pressure, temperature-adjusting device, pressure adjusting range between 0-10 megapascal or 1-7 megapascal it
Between, temperature range is between 0-500 degrees Celsius.
4. a kind of high-throughput sieve sample preparation system available for sieve sample screening, it is characterised in that：It includes
Free-standing crystallization system and cleaning filtration system；Wherein free-standing crystallization system includes the reactor of several independent controls, often
The preparation condition of sieve sample in one reactor is independently of the preparation condition of the sieve sample in other reactors, cleaning
Filtration system, which can be provided, to be cleaned, filtered and is dried to the sieve sample preliminarily formed, so as to complete molecular sieve sample
The preparation of product.
5. high throughput sieve sample preparation system as claimed in claim 4, it is characterised in that：Wherein free-standing crystallization system
The independent control that can be provided each reactor includes pressure control, the control of temperature and time, independent stirring control, in real time
At least one of control for controlling, detecting in real time of charging or sampling.
6. high throughput sieve sample preparation system as claimed in claim 4, it is characterised in that：Wherein described reactor setting
Stirring, detection device, reaction module are provided with pressure, temperature-adjusting device, pressure adjusting range between 0-10 megapascal or
Between 0-6 megapascal, temperature range is between 0-500 degrees Celsius.
7. high throughput sieve sample preparation system as described in claim 1 or 4, it is characterised in that：It is still further comprised
Sample analysis system, wherein sample analysis system are one kind in X-ray diffraction system or X-ray powder diffraction instrument.
8. high throughput sieve sample preparation system as described in claim 1 or 4, it is characterised in that：It is still further comprised
Data processing system can provide data processing, phasor and model analysis.
9. a kind of workflow of the sieve sample research/development platform of high throughput includes design, the raw material of sieve sample
Prepare, prepared by sample library, sieve sample synthesizes, six comprising modules of sample analysis and data analysis.
10. the workflow of high throughput sieve sample research/development platform as claimed in claim 9, it is characterised in that：Wherein exist
Sieve sample synthesis module can use high-throughput techniques, carry out multistage screening；Wherein described multistage screening includes primary sieve
Choosing, two level screening, three level screen, enlarged experiment screening；Screening system wherein selected by primary screener be such as claim 1 and
Or the high-throughput sieve sample preparation system described in 4.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111437780A (en) * | 2020-03-20 | 2020-07-24 | 安徽大学 | Hydrothermal solvent heat parallel synthesis device |
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Application publication date: 20180710 |