CN105741357A - Method of reproducing molecular sieve crystallization processes and describing appearances - Google Patents
Method of reproducing molecular sieve crystallization processes and describing appearances Download PDFInfo
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Abstract
The invention relates to a method of reproducing molecular sieve crystallization processes and describing appearances, comprising the steps of: first, screening and establishing primitive cells; second, establishing a crystal growth dynamic model; third, obtaining crystal surface primitive cell position data; and fourth, drafting a molecular sieve crystal appearance graph according to the crystal surface primitive cell position data. The method utilizes a cellular automation and random theoretical method and a multi-core computer string/parallel calculating mode to dynamically describe molecular sieve crystal growth processes, and draft molecular sieve appearances according with industrial molecular sieve real characteristics and having different resolutions, and possesses important guiding significance and wide applicability in molecular sieve crystallization processes and appearance reconstruction.
Description
Technical field
The present invention relates to a kind of crystallization process reproducing molecular sieve the method describing its exterior appearance, belong to crystal-type catalysis material structural research technical field.
Background technology
For a long time, molecular sieve is as industrial catalyst, and especially the important carrier of Cracking catalyst is industrially widely used.But, for the study mechanism of associated catalytic process so far still in the primary stage.Its reason root on the one hand is in the extremely complicated property of catalytic process essence；The study model that classical study mechanism adopts on the other hand is imaginary desirable cell configuration, and this desirable cell configuration has quite huge difference with industrial molecular sieve reality appearance structure, thus causing the disconnection of theoretical research and practical application, research effect cannot really be applied.
Along with improving constantly of catalysis material analysis level and modern computer computing capability, research worker can observe and study the pattern of catalysis material itself, structure and nature and characteristic on bigger spatial and temporal scales.
CN103575734A discloses the three-dimensional imaging of crystal three-dimensional crystal face growth kinetics and measures system, it is possible to realize the reproduction of 3D crystal formation.The method establishes the Three Dimensional Reconfiguration of a kind of crystal growing surface microstructure observation system comprising scope and different angles crystal two-dimensional signal.But the program does not provide the crystal growth mathematical model of a class system；And the crystal yardstick that reconstructed by equipment observation station is relatively large, is typically in 100 microns；Additionally, the crystal outward appearance reconstructed is generally fairly simple, when crystal outward appearance is extremely complex, the probability that the Two-Dimensional Reconstruction involved by this invention calculates the reconstruct that makes a mistake is bigger.
CN101561401A discloses a kind of method utilizing laser digital phase shift interference system device real-time monitored water solublity crystal, organic crystal growing surface micro structure.The change of interference fringe produced by the optical interference phenomena of this invention application crystal carrys out indirect measurement and observation station relates to the growth behavior of crystal.But the program does not provide the crystal growth mathematical model of such system；Secondly, He-Ne laser wavelength given by embodiment is 632.8nm, the crystal yardstick that restriction which of associated laser half-wavelength can be measured should be not less than about 320nm, therefore for short grained nano crystals, is difficult to find the high-frequency electromagnetic wave ray that can produce stable interference.
Summary of the invention
For the defect that technique scheme exists, spy of the present invention proposes a kind of crystallization process reproducing molecular sieve the method describing its exterior appearance, and the mode calculated by high-density analog is established and more conformed to the exterior appearance feature that industrial molecular sieve is actual.By each crystalloid that dimensional variation is relatively big and outward appearance is complicated that the method for the invention can reconstruct, and then the research for deeply carrying out catalysis behavior provides important evidence.
To achieve these goals, the present invention adopts the following technical scheme that
A kind of crystallization process reproducing molecular sieve the method describing its exterior appearance, as Figure 1-3, comprise the steps:
One, the screening of primitive unit cell and establishment:
Two, crystal growth Dynamic Model；
Three, the position data of plane of crystal primitive unit cell is obtained；
Four, according to the position data of surface primitive unit cell, the exterior appearance figure of molecular sieve crystal is drawn.
In the above-mentioned methods, step one includes:
1) construction unit repeated in molecular sieve structure is analyzed, lists multiple basic structural unit that may be present；
2) analytical procedure 1) in basic structural unit, filter out construction unit symmetry Dot Cellular Automata form high, the follow-up succinct basic structural unit primitive unit cell as crystal growth.
In the above-mentioned methods, step 2 includes: according to Dot Cellular Automata Mode Equation, forms dot matrix with selected primitive unit cell for a stacking, obtains the mathematic(al) mode of crystal growing process Dynamic profiling；
Wherein, described Dot Cellular Automata Mode Equation is deterministic type Dot Cellular Automata Mode Equation or probabilistic type Dot Cellular Automata Mode Equation, it is preferable that probabilistic type Dot Cellular Automata Mode Equation.
Being applied to each point by transformation rule, will there is the evolution of automat in the state of this point.These rules determine the state of lattice lattice point；Here it is assumed that its state of each lattice-site is the function of the contiguous lattice point state of its previous time point, Dot Cellular Automata is with discrete time step development and develops.So through an interval, the state variable value of all nodes be updated simultaneously.
In the Dot Cellular Automata that the present invention relates to, it is specifically determined by a set of probabilistic transformation rule that the local of adjacent lattice seat interacts.When the time (t), for the state variable value ζ of certain some jj, will by the adjacent states variate-value ζ of current state previous time point (t-Δ t)j+1, ζj+2, ζj+3And ζj+4Determine.
Adopt linear transformation rule as follows at this:
For state variable ζT, j,
As time t, j point is occupied
As time t, j point is not occupied
Total status number for moment t surface point to be generated is:
Wherein to be that surface is all to be generated count out n, and the generating probability of each point to be generated is:
Produce the random number P between a 0-1,
If Rt,j<P≤Rt+1,j
So
Otherwise
In the above-mentioned methods, step 3 includes:
1) adopt multi-core computer serial/parallel row computational methods that crystal growth behavior is carried out numerical simulation the mathematic(al) mode established；Calculate molecular sieve average dimension in real time, Mobile state simulation is grown into for molecular sieve and calculates, calculate the position coordinate data of newly-increased primitive unit cell；
Wherein, in the described serial/parallel row computational methods of multi-core computer, parallel computation number of unit is not less than 2, it is preferable that more than 4 computing units.
With the coordinate position of initial primitive unit cell for benchmark, randomly select a position according to docking form, as next primitive unit cell, position occurs；After introducing next primitive unit cell, there are two primitive unit cells simultaneously in system；The new system comprising two primitive unit cells is updated the positional information of the record each primitive unit cell of new system, new system comprises the position that six new primitive unit cells are likely to occur, according still further to probability calculation next primitive unit cell, position occurs, and record and update the position coordinates of each primitive unit cell of system comprising three primitive unit cells, calculating process records the surface primitive unit cell positional information of system simultaneously；By that analogy, that goes round and begins again repeats above-mentioned calculating process, until the average crystalline size of simulated system gained reaches target size, then stops calculating.
2) acquired primitive unit cell spatial point data are updated, calculate the position data obtaining molecular sieve crystal surface primitive unit cell.
In the above-mentioned methods, step 4 includes: the position data of surface primitive unit cell obtained is carried out surface interpolation, draws not in the same time, the molecular sieve exterior appearance figure of different resolution；
Wherein, described surface interpolation adopts spline surface mode, it is preferable that cubic spline mode, B-spline mode or U, V system three-dimensional batten mode.
Compared with prior art, the inventive method has the advantage that
1, the method for the invention can produce more to meet the exterior appearance of industrial molecular sieve actual look shape characteristic, especially that the molecular sieve system of industrial commercially valuable non-low limited synthesis condition synthesis is all the more so.
2, the molecular sieve system described in this method can carry out the probabilistic type continuation of aperiodic, non-determined type, for instance step, dislocation, crystal edge, crystal angle, cusp etc. exist the site, space of higher catalytic activity；And the molecular sieve system involved by traditional approach can only carry out periodically, deterministic continuation.By contrast, the involved molecular sieve system produced of this method more generality and universality.
3, the molecular sieve system described by this method can carry out the multiresolution analysis of different scale by mathematical way, and then can contrast with the Electron Microscope images system of different resolution, the crystal complicated for outward appearance also is able to realize accurate simulation, and this is that conventional molecular sieve tectonic system cannot be reached.
4, crystal simulation yardstick involved in the present invention from Ethylmercurichlorendimide level to decimeter grade, can adapt to most crystal growth size.
The inventive method utilizes Dot Cellular Automata and random theory method, use the serial/parallel row computation schema of multi-core computer, the growth course of Dynamic profiling molecular sieve crystal, and draw out the molecular sieve exterior appearance with different resolution meeting industrial molecular sieve real features, growth course and pattern reconstruct for molecular sieve crystal have great directive significance and wide applicability.
Accompanying drawing explanation
Fig. 1 is the crystallization process of reproduction molecular sieve of the present invention and describes the schematic flow sheet of method of its exterior appearance.
Fig. 2 is the computing block diagram of the molecular sieve dynamic growth of first and second step in the method for the invention.
Fig. 3 is the computing block diagram of the molecular sieve surface pattern description of the 3rd and the 4th step in the method for the invention.
Fig. 4 is all kinds of primitive unit cells and the selection primitive cell structure schematic diagram of FAU type molecular sieve in the embodiment of the present invention 1.
Fig. 5 is four kinds of docking forms of the primitive unit cell of FAU molecular sieve in the embodiment of the present invention 1.
Fig. 6 is the exterior appearance of different time in the embodiment of the present invention 1 Middle molecule sieve growth course.
Fig. 7 is micron-level molecular sieve exterior appearance obtained in the embodiment of the present invention 1.
Fig. 8 is scanning electron microscope (SEM) photo of technical grade NaY molecular sieve.
Fig. 9 is Fig. 8 and Fig. 7 molecular sieve image comparison figure obtained.
Figure 10 is the descriptive model of tradition NaY molecular sieve crystal structure.
Detailed description of the invention
Below by the specific embodiment crystallization process to described reproduction molecular sieve and describe the method for its exterior appearance and be described further.
Following example are used for illustrating the present invention, but are not limited to the scope of the present invention.
Embodiment 1
Below for technical grade NaY molecular sieve, describe the crystallization process of FAU molecular sieve the method describing its exterior appearance in detail, comprise the steps:
One, the screening of primitive unit cell and establishment in FAU molecular sieve crystal:
1) construction unit of repeatable appearance in technical grade NaY molecular sieve structure is analyzed, there is the multiple basic structural unit of A, B, C, D, E etc. as shown in Figure 4；
2) factor such as complexity and relevant calculating intensity of the symmetry of primitive unit cell self, follow-up automat algorithm is considered, successively the selection of primitive unit cell is analyzed, wherein can using the silica in molecular sieve or aluminum-oxygen tetrahedron as primitive unit cell, as schemed shown in A, also the four-membered ring that can silica or aluminum-oxygen tetrahedron be formed or hexatomic ring are as primitive unit cell, as schemed shown in B or figure C, but such primitive unit cell is smaller, and follow-up automat equation form is complicated, the relatively die of consumption calculations resource is not easily as waiting to select primitive unit cell.Further, it is also possible to select the big cluster of FAU molecular sieve as shown in figure D as primitive unit cell, although reducing follow-up automat equation complexity, but there are two significant drawbacks: first, the interaction between primitive unit cell calculates complexity；Secondly, the symmetry of primitive unit cell system is relatively low.Considering factors above, select figure E basic primitive unit cell grow as automat, referred to as β cage, it is simultaneously satisfied has the advantage such as higher-symmetry and more succinct Dot Cellular Automata form.
Two, FAU molecular sieve crystal Dynamic Growth Models is set up:
According to probabilistic type Dot Cellular Automata Mode Equation, form dot matrix with selected primitive unit cell for a stacking, obtain the mathematic(al) mode of crystal growing process Dynamic profiling；
Particularly as follows: have four kinds of docking form A, B, C and D between the primitive unit cell determined of step one, as shown in Figure 5.In Fig. 4, E primitive unit cell is growth primitive unit cell, then primitive unit cell number this structures more many being adjacent are more stable, and to occur in the probability in crystal also more big for this structure simultaneously.Therefore, it can assert that in crystal growing process, A, B, C and D tetra-kinds docking Form generation likelihood ratio is 1:2:3:4.
Being applied to each point by transformation rule, will there is the evolution of automat in the state of this point.These rules determine the state of lattice lattice point；Here it is assumed that its state of each lattice-site is the function of the contiguous lattice point state of its previous time point, Dot Cellular Automata is with discrete time step development and develops.So through an interval, the state variable value of all nodes be updated simultaneously.
In the Dot Cellular Automata that the present invention relates to, it is specifically determined by a set of probabilistic transformation rule that the local of adjacent lattice seat interacts.When the time (t), for the state variable value ζ of certain some jj, will by the adjacent states variate-value ζ of current state previous time point (t-Δ t)j+1, ζj+2, ζj+3And ζj+4Determine.
Adopt linear transformation rule as follows at this:
For state variable ζT, j,
As time t, j point is occupied
As time t, j point is not occupied
Total status number for moment t surface point to be generated is:
Wherein to be that surface is all to be generated count out n, and the generating probability of each point to be generated is:
Produce the random number P between a 0-1,
If Rt,j<P≤Rt+1,j
So
Otherwise
Three, the position data of plane of crystal primitive unit cell is obtained；
Adopt multi-core computer serial/parallel row computational methods that crystal growth behavior is carried out numerical simulation the mathematic(al) mode established；Calculate molecular sieve average dimension in real time, Mobile state simulation is grown into for molecular sieve and calculates, calculate the position coordinate data of newly-increased primitive unit cell；
Particularly as follows: with the coordinate position of initial primitive unit cell for benchmark, randomly select a position according to docking form (in Fig. 5 D structure) in four positions being adjacent, as next primitive unit cell, position occur.After introducing next primitive unit cell, there are two primitive unit cells simultaneously in system；The new system comprising two primitive unit cells is updated the positional information of the record each primitive unit cell of new system, new system comprises the position that six new born of the same parents are likely to occur, according still further to probability calculation next primitive unit cell, position occurs, and record and update the position coordinates of each primitive unit cell of system comprising three primitive unit cells, by that analogy, that goes round and begins again repeats above-mentioned calculating process, until the average crystalline size of simulation gained is 120nm, then stops calculating.
The surface primitive unit cell positional information of record system.
Four, according to the position data of gained surface primitive unit cell, the exterior appearance figure of molecular sieve crystal is drawn:
Obtain the positional information of the system surface primitive unit cell of record in calculating process, adopt cubic spline mode to carry out surface interpolation, draw not in the same time, the molecular sieve exterior appearance figure of different resolution, as shown in Figure 6.
Finally give sodium meter level FAU molecular sieve surface structure, as shown in Figure 7.
Comparative example 1
Fig. 8 is scanning electron microscope (SEM) photo of technical grade NaY molecular sieve.Molecular sieve corresponding for black box in Fig. 8 is contrasted with Fig. 7 molecular sieve appearance images obtained, namely shown in Fig. 9.Therefrom it appeared that the real system simulating the acquired molecular sieve body exterior appearance of calculating and substance feature and industrial molecular sieve crystal is very much like.
Comparative example 2
Adopting certain industrial molecular with FAU structure type codes that traditional approach obtains to sieve original crystalline structure, comprise T atom and the oxygen atom being attached thereto in its structure, its structure type is also ball-and-stick model, and concrete structure is as shown in Figure 10.
For the describing mode of traditional NaY molecular sieve, being merely able to carry out Cubic periodic extension with the structural system shown in Figure 10, the crystal structure exterior appearance that it obtains is a cube form.Step, dislocation, crystal edge and crystal angle that real industrial NaY molecular sieve has etc. cannot be embodied complicated and real form.
From the foregoing, say from space angle, the molecular sieve system that the method for the invention generates has the similarity degree very big with real industrial molecular sieve system.Compare conventional molecular sieve nest system building method mutually, the present invention can describe the various non-canonical of true molecular sieve nest system, acyclic row looks with more large scale, bigger resolution, for instance step, dislocation, crystal edge, crystal angle, cusp etc. exist the site, space of higher catalytic activity；From time angle, this method can describe the real-time growth course of molecular sieve system, has great contribution for studying molecular simulation further.
Although, above the present invention is described in detail with a general description of the specific embodiments, but on basis of the present invention, it is possible to it is made some modifications or improvements, and this will be apparent to those skilled in the art.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, belong to the scope of protection of present invention.
Claims (8)
1. one kind reproduces the crystallization process of molecular sieve and describes the method for its exterior appearance, it is characterised in that comprise the steps:
One, the screening of primitive unit cell and establishment:
Two, crystal growth Dynamic Model；
Three, the position data of plane of crystal primitive unit cell is obtained；
Four, according to the position data of surface primitive unit cell, the exterior appearance figure of molecular sieve crystal is drawn.
2. reproduce the crystallization process of molecular sieve according to claim 1 and describe the method for its exterior appearance, it is characterised in that described step one includes:
1) construction unit repeated in molecular sieve structure is analyzed, lists multiple basic structural unit that may be present；
2) analytical procedure 1) in basic structural unit, filter out construction unit symmetry Dot Cellular Automata form high, the follow-up succinct basic structural unit primitive unit cell as crystal growth.
3. reproduce the crystallization process of molecular sieve according to claim 1 and describe the method for its exterior appearance, it is characterized in that, described step 2 includes: according to Dot Cellular Automata Mode Equation, forms dot matrix with selected primitive unit cell for a stacking, obtains the mathematic(al) mode of crystal growing process Dynamic profiling.
4. reproduce the crystallization process of molecular sieve according to claim 3 and describe the method for its exterior appearance, it is characterised in that described Dot Cellular Automata Mode Equation is deterministic type Dot Cellular Automata Mode Equation or probabilistic type Dot Cellular Automata Mode Equation.
5. reproduce the crystallization process of molecular sieve according to claim 1 and describe the method for its exterior appearance, it is characterised in that described step 3 includes:
1) adopt multi-core computer serial/parallel row computational methods that crystal growth behavior is carried out numerical simulation the mathematic(al) mode established；Calculate molecular sieve average dimension in real time, Mobile state simulation is grown into for molecular sieve and calculates, calculate the position coordinate data of newly-increased primitive unit cell；
2) acquired primitive unit cell spatial point data are updated, calculate the position data obtaining molecular sieve crystal surface primitive unit cell.
6. reproduce the crystallization process of molecular sieve according to claim 5 and describe the method for its exterior appearance, it is characterised in that in the described serial/parallel row computational methods of multi-core computer, parallel computation number of unit is not less than 2, it is preferable that more than 4 computing units.
7. reproduce the crystallization process of molecular sieve according to claim 1 and describe the method for its exterior appearance, it is characterized in that, described step 4 includes: the position data of surface primitive unit cell obtained is carried out surface interpolation, draws not in the same time, the molecular sieve exterior appearance figure of different resolution.
8. reproduce the crystallization process of molecular sieve according to claim 7 and describe the method for its exterior appearance, it is characterised in that described surface interpolation adopts spline surface mode.
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| CN1866464A (en) * | 2005-05-16 | 2006-11-22 | 中国科学院半导体研究所 | Mirror charge effect quantum cellular automation making method |
| CN101591729A (en) * | 2009-06-19 | 2009-12-02 | 东北大学 | The method of structure evolution of austenite dynamic recrystallization in the prediction thermal deformation of plate-strip steel |
| CN102930143A (en) * | 2012-10-11 | 2013-02-13 | 清华大学 | Method for determining incident angle of particles in three-dimensional cellular model etching process |
| WO2014034964A3 (en) * | 2012-08-31 | 2014-06-19 | Kabushiki Kaisha Toshiba | Method and system for predicting material structure |
| CN103993138A (en) * | 2014-05-29 | 2014-08-20 | 东北大学 | Method for predicting martensite structure evolution in high-strength plastic product steel quenching |
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- 2014-12-06 CN CN201410743302.8A patent/CN105741357B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1866464A (en) * | 2005-05-16 | 2006-11-22 | 中国科学院半导体研究所 | Mirror charge effect quantum cellular automation making method |
| CN101591729A (en) * | 2009-06-19 | 2009-12-02 | 东北大学 | The method of structure evolution of austenite dynamic recrystallization in the prediction thermal deformation of plate-strip steel |
| WO2014034964A3 (en) * | 2012-08-31 | 2014-06-19 | Kabushiki Kaisha Toshiba | Method and system for predicting material structure |
| CN102930143A (en) * | 2012-10-11 | 2013-02-13 | 清华大学 | Method for determining incident angle of particles in three-dimensional cellular model etching process |
| CN103993138A (en) * | 2014-05-29 | 2014-08-20 | 东北大学 | Method for predicting martensite structure evolution in high-strength plastic product steel quenching |
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