CN105741357B - A method of it reproducing the crystallization process of molecular sieve and describes its exterior appearance - Google Patents
A method of it reproducing the crystallization process of molecular sieve and describes its exterior appearance Download PDFInfo
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Abstract
The present invention relates to a kind of crystallization process reproducing molecular sieve and the methods for describing its exterior appearance, include the following steps：One, the screening and establishment of primitive unit cell：Two, crystal growth Dynamic Model；Three, the position data of plane of crystal primitive unit cell is obtained；Four, the position data according to surface primitive unit cell, draws the exterior appearance figure of molecular sieve crystal.The method of the present invention utilizes Dot Cellular Automata and random theory method, pattern is calculated with the serial/parallel row of multi-core computer, the growth course of Dynamic profiling molecular sieve crystal, and the molecular sieve exterior appearance with different resolution for meeting industrial molecular sieve real features is drawn out, the growth course and pattern reconstruct for molecular sieve crystal have great directive significance and wide applicability.
Description
Technical field
The present invention relates to a kind of crystallization process reproducing molecular sieve and the methods for describing its exterior appearance, belong to crystal-type and urge
Change material structure studying technological domain.
Background technology
For a long time, molecular sieve is industrially wide as the important carrier of industrial catalyst, especially Cracking catalyst
For application.However, for associated catalytic process mechanism study so far still in the primary stage.Its reason one side root is in urging
The extremely complicated property of change process essence；On the other hand research model used by classical mechanism study is imaginary ideal structure cell knot
Structure, and this ideal cell configuration has quite huge difference with the real appearance structure of industrial molecular sieve, to cause theory
The disconnection of research and practical application, research effect are unable to get real application.
With the continuous improvement of catalysis material analysis level and modern computer computing capability, researcher can be more
The pattern of catalysis material itself, structure and nature and characteristic are observed and studied on big spatial and temporal scales.
CN103575734A discloses the three-dimensional imaging measurement system of crystal three-dimensional crystal face growth kinetics, can realize 3D
The reproduction of crystal form.This method establishes a kind of crystal growing surface microstructure observation system and different angle comprising observation device
The Three Dimensional Reconfiguration of crystal two-dimensional signal.But the program does not provide the crystal growth mathematical model of a kind of system；And pass through
The crystal scale of equipment observation station reconstruct is relatively large, generally in 100 microns；In addition, the crystal appearance reconstructed is general
It is fairly simple, when crystal appearance is extremely complex, Two-Dimensional Reconstruction involved by the invention calculate occur the probability of mistake reconstruct compared with
Greatly.
CN101561401A disclose it is a kind of using laser digital phase shift interference system device observe in real time water solubility crystal,
The method of organic crystal growing surface micro-structure.The change of interference fringe caused by the optical interference phenomena of the invention application crystal
Change the growth behavior for coming indirect measurement and the involved crystal of observation.But the program does not provide the crystal growth mathematics of such system
Model；Secondly, the He-Ne laser wavelengths given by embodiment are 632.8nm, limitation which of associated laser half-wavelength
The crystal scale that can be measured should be not less than 320nm or so, therefore for short grained nano crystals, can it is difficult to find
Generate the high-frequency electromagnetic wave ray for stablizing interference.
Invention content
Defect existing for scheme in view of the above technology, a kind of crystallization process reproducing molecular sieve of the special proposition of the present invention and description
The method of its exterior appearance is established by way of high-density analog calculating and is more in line with the actual exterior appearance of industrial molecular sieve
Feature.Each crystalloid that the dimensional variation that the method can reconstruct through the invention is larger and appearance is complicated, and then be deep
The research for carrying out catalysis behavior provides important evidence.
To achieve the goals above, the present invention adopts the following technical scheme that：
A method of it reproducing the crystallization process of molecular sieve and describes its exterior appearance, as shown in Figs. 1-3, including it is as follows
Step：
One, the screening and establishment of primitive unit cell：
Two, crystal growth Dynamic Model；
Three, the position data of plane of crystal primitive unit cell is obtained；
Four, the position data according to surface primitive unit cell, draws the exterior appearance figure of molecular sieve crystal.
In the above-mentioned methods, step 1 includes：
1) structural unit repeated in molecular sieve structure is analyzed, lists a variety of basic structures that may be present
Unit；
2) analytical procedure 1) in basic structural unit, filter out that structural unit symmetry is high, follow-up Dot Cellular Automata form
Primitive unit cell of the succinct basic structural unit as crystal growth.
In the above-mentioned methods, step 2 includes：It is point stacking shape with selected primitive unit cell according to Dot Cellular Automata Mode Equation
At dot matrix, the mathematic(al) mode of crystal growing process Dynamic profiling is obtained；
Wherein, the Dot Cellular Automata Mode Equation is that deterministic type Dot Cellular Automata Mode Equation or probabilistic type primitive unit cell are automatic
Machine Mode Equation, preferred probability type Dot Cellular Automata Mode Equation.
It is applied to each point by transformation rule, the evolution of automatic machine will occur for the state of the point.These rules determine
The state of lattice lattice point；Here it is assumed that its state of each lattice-site is function of its previous time point adjacent to lattice point state, primitive unit cell
Automatic machine is to walk development with discrete time and develop.So by a time interval, it be to the state variable value of all nodes
It updates simultaneously.
In Dot Cellular Automata of the present invention, the local interaction of adjacent lattice seat is by a set of probabilistic change
It changes regular specific determining.In the time (t), to the state variable value ζ of Mr. Yu's point jj, will be by current state previous time point (t-
The state variable value ζ of four close positions of Δ t)j1, ζj2, ζj3And ζj4It determines.
Use linear transformation rule as follows herein：
For state variable ζT, jFor,
As time t, j points are occupied
As time t, j points are not occupied
Total status number for moment t surface point to be generated is：
Wherein n be surface it is all it is to be generated count out, the generating probability of each point to be generated is：
The random number P between a 0-1 is generated,
If Rt,j＜ P≤Rt+1,j
So
Otherwise
In the above-mentioned methods, step 3 includes：
1) numerical value is carried out to crystal growth behavior using the serial/parallel row computational methods of multi-core computer to established mathematic(al) mode
Simulation；Molecular sieve average dimension is calculated in real time, molecular sieve is grown and carries out dynamic analog calcutation, calculates the position for increasing primitive unit cell newly
Coordinate data；
Wherein, in the serial/parallel row computational methods of multi-core computer, parallel computation number of unit is excellent not less than 2
Select 4 computing units or more.
On the basis of the coordinate position of initial primitive unit cell, a position is randomly selected as next primitive unit cell according to docking form
There is position；After introducing next primitive unit cell, there are two primitive unit cells simultaneously in system；New system comprising two primitive unit cells is updated
The location information of each primitive unit cell of new system is recorded, new system includes the position that six new primitive unit cells are likely to occur, according still further to probability meter
It calculates next primitive unit cell and position occurs, and record and update the position coordinates of each primitive unit cell of system comprising three primitive unit cells, calculating
Record the surface primitive unit cell location information of system simultaneously in the process；And so on, the above-mentioned calculating process of repetition in cycles, until
Average crystalline size obtained by simulated system reaches target size, then stops calculating.
2) acquired primitive unit cell space point data is updated, calculates the positional number for obtaining molecular sieve crystal surface primitive unit cell
According to.
In the above-mentioned methods, step 4 includes：Surface interpolation is carried out to the position data of the surface primitive unit cell of acquisition, is drawn not
In the same time, the molecular sieve exterior appearance figure of different resolution；
Wherein, the surface interpolation uses spline surface mode, preferably cubic spline mode, B-spline mode or U, V system
Three-dimensional batten mode.
Compared with prior art, the method for the present invention has the following advantages：
1, the method for the invention can generate the exterior appearance for more meeting industrial molecular sieve actual look shape characteristic, especially
It is even more so to the molecular sieve system of industrial commercially valuable non-low limited synthesis condition synthesis.
2, the molecular sieve system described in this method can carry out the probabilistic type continuation of aperiodic, non-determined type, such as
There are the space sites of higher catalytic activity for step, dislocation, crystal edge, crystal angle, cusp etc.；And the molecular sieve involved by traditional approach
System can only carry out periodical, deterministic continuation.In contrast, the involved molecular sieve system generated of this method is more general
Property and generality.
3, molecular sieve system described in this method can carry out the multiresolution analysis of different scale by mathematical way, into
And can be compared with the Electron Microscope images system of different resolution, standard can also be realized for the crystal of appearance complexity
Really simulation, this, which is conventional molecular sieve tectonic system, to reach.
4, crystal simulation scale according to the present invention can adapt to most crystal growth rulers from Ethylmercurichlorendimide grade to decimeter grade
It is very little.
The method of the present invention utilizes Dot Cellular Automata and random theory method, and pattern is calculated with the serial/parallel row of multi-core computer,
The growth course of Dynamic profiling molecular sieve crystal, and draw out meet industrial molecular sieve real features with different resolution
Molecular sieve exterior appearance, growth course and pattern reconstruct for molecular sieve crystal have great directive significance and widely fit
The property used.
Description of the drawings
Fig. 1 is the flow signal of the crystallization process of the present invention for reproducing molecular sieve and the method that describes its exterior appearance
Figure.
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 third and four steps in the method for the invention.
Fig. 4 is all kinds of primitive unit cells and selection primitive cell structure schematic diagram of FAU type molecular sieves in the embodiment of the present invention 1.
Fig. 5 is four kinds of docking forms of the primitive unit cell of FAU molecular sieves in the embodiment of the present invention 1.
Fig. 6 is the exterior appearance of different time in molecular sieve growth course in the embodiment of the present invention 1.
Fig. 7 is obtained nano-class molecular sieve exterior appearance 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 the molecular sieve image comparison figure that Fig. 8 and Fig. 7 is obtained.
Figure 10 is the descriptive model of traditional NaY molecular sieve crystal structure.
Specific implementation mode
The crystallization process for reproducing molecular sieve and the method that describes its exterior appearance are done below by specific embodiment
Further instruction.
The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention..
Embodiment 1
Below by taking technical grade NaY molecular sieve as an example, the crystallization process of FAU molecular sieves is described in detail and describes its exterior appearance
Method, include the following steps：
One, in FAU molecular sieve crystals primitive unit cell screening and establishment：
1) it analyzes repeating the structural unit occurred in technical grade NaY molecular sieve structure, there are as shown in Figure 4
A variety of basic structural units such as A, B, C, D, E；
2) consider symmetry, the complexity of follow-up automatic machine algorithm and relevant calculating intensity etc. of primitive unit cell itself because
Element successively analyzes the selection of primitive unit cell, wherein can using in molecular sieve silica or aluminum-oxygen tetrahedron as primitive unit cell, such as scheme A
Shown, the four-membered ring or hexatomic ring that can also form silica or aluminum-oxygen tetrahedron are as primitive unit cell, as shown in figure B or figure C, but such
Primitive unit cell size is smaller, and follow-up automatic machine equation form is complicated, and consumption calculations resource is not easy compared with die as primitive unit cell to be selected.This
Outside, it is also an option that the big cluster of FAU molecular sieves is as primitive unit cell as shown in figure D, although reducing follow-up automatic machine equation complexity journey
Degree, however there are two significant drawbacks：First, the interaction between primitive unit cell calculates complicated；Secondly, the symmetry of primitive unit cell system
It is relatively low.Consider factors above, the basic primitive unit cell for selecting figure E to be grown as automatic machine, referred to as β cages are full simultaneously
Foot has many advantages, such as higher-symmetry and more succinct Dot Cellular Automata form.
Two, FAU molecular sieve crystals Dynamic Growth Models are established：
According to probabilistic type Dot Cellular Automata Mode Equation, it is that point stacking forms dot matrix with selected primitive unit cell, obtains crystal life
The mathematic(al) mode of growth process Dynamic profiling；
Specially：There are four types of form A, B, C and D is docked between the primitive unit cell that step 1 determines, as shown in Figure 5.With E in Fig. 4
Primitive unit cell is growth primitive unit cell, then the more structures of primitive unit cell number adjacent thereto are more stable, while the structure appears in crystal
Probability it is also bigger.Therefore, it can be assumed that tetra- kinds of docking form generating probability ratios of A, B, C and D are 1 in crystal growing process：
2：3：4.
It is applied to each point by transformation rule, the evolution of automatic machine will occur for the state of the point.These rules determine
The state of lattice lattice point；Here it is assumed that its state of each lattice-site is function of its previous time point adjacent to lattice point state, primitive unit cell
Automatic machine is to walk development with discrete time and develop.So by a time interval, it be to the state variable value of all nodes
It updates simultaneously.
In Dot Cellular Automata of the present invention, the local interaction of adjacent lattice seat is by a set of probabilistic change
It changes regular specific determining.In the time (t), to the state variable value ζ of Mr. Yu's point jj, will be by current state previous time point (t-
The state variable value ζ of four close positions of Δ t)j1, ζj2, ζj3 and ζj4 determine.
Use linear transformation rule as follows herein：
For state variable ζT, jFor,
As time t, j points are occupied
As time t, j points are not occupied
Total status number for moment t surface point to be generated is：
Wherein n be surface it is all it is to be generated count out, the generating probability of each point to be generated is：
The random number P between a 0-1 is generated,
If Rt,j＜ P≤Rt+1,j
So
Otherwise
Three, the position data of plane of crystal primitive unit cell is obtained；
Numerical-Mode is carried out to crystal growth behavior using the serial/parallel row computational methods of multi-core computer to established mathematic(al) mode
It is quasi-；Molecular sieve average dimension is calculated in real time, molecular sieve is grown and carries out dynamic analog calcutation, and the position that calculating increases primitive unit cell newly is sat
Mark data；
Specially：On the basis of the coordinate position of initial primitive unit cell, according to docking form in four positions adjacent thereto
(D structures in Fig. 5) randomly selects a position and position occurs as next primitive unit cell.After introducing next primitive unit cell, system is simultaneously
There are two primitive unit cells；The location information of the record each primitive unit cell of new system, new body are updated to the new system comprising two primitive unit cells
There is position according still further to the next primitive unit cell of probability calculation, and records and update in the position that system is likely to occur comprising six new Yuan born of the same parents
Include the position coordinates of each primitive unit cell of the system of three primitive unit cells, and so on, the above-mentioned calculating process of repetition in cycles, until
The average crystalline size of simulation gained is 120nm, then stops calculating.
The surface primitive unit cell location information of record system.
Four, the position data according to gained surface primitive unit cell, draws the exterior appearance figure of molecular sieve crystal：
The location information for obtaining the system surface primitive unit cell recorded in calculating process carries out curved surface using cubic spline mode and inserts
Value, draw different moments, different resolution molecular sieve exterior appearance figure, as shown in Figure 6.
Nanoscale FAU molecular sieve surface structures are finally obtained, as shown in Figure 7.
Comparative example 1
Fig. 8 is scanning electron microscope (SEM) photo of technical grade NaY molecular sieve.By corresponding point of black box in Fig. 8
The molecular sieve appearance images that son sieve is obtained with Fig. 7 are compared, i.e., shown in Fig. 9.Therefrom it can be found that simulating acquired in calculating
The real system that molecular sieve body exterior appearance sieves crystal with substance feature with industrial molecular is very much like.
Comparative example 2
Original crystalline structure is sieved using certain industrial molecular with FAU structure type codes that traditional approach obtains,
The oxygen atom for including T atom in structure and being attached thereto, structure type are also ball-and-stick model, and concrete structure is as shown in Figure 10.
For the describing mode of traditional NaY molecular sieve, it is merely able to carry out Cubic week with structural system shown in Fig. 10
Phase continuation, the crystal structure exterior appearance obtained are a cube forms.Real industrial NaY molecular sieve can not be embodied to be possessed
Step, dislocation, crystal edge and crystal angle etc. be complicated and true form.
It can be seen from the above, for space angle, the molecular sieve system that the method for the invention generates has and true work
The prodigious similarity degree of industry molecular sieve system.Compared to than conventional molecular sieve nest system building method, the present invention can with more large scale,
Bigger resolution ratio describes the various non-canonicals of true molecular sieve nest system, acyclic row looks, such as step, dislocation, crystal edge, crystalline substance
There are the space sites of higher catalytic activity for angle, cusp etc.；For time angle, this method can describe molecular sieve system
Real-time growth course has greatly contribution for further studying molecular simulation.
Although above the present invention is described in detail with a general description of the specific embodiments,
On the basis of the present invention, it can be made some modifications or improvements, this will be apparent to those skilled in the art.Cause
This, these modifications or improvements, belong to the scope of protection of present invention without departing from theon the basis of the spirit of the present invention.
Claims (8)
1. a kind of crystallization process reproducing molecular sieve and the method for describing its exterior appearance, which is characterized in that include the following steps：
One, the screening and establishment of primitive unit cell：
Two, crystal growth Dynamic Model；
Three, the position data of plane of crystal primitive unit cell is obtained；
Four, the position data according to surface primitive unit cell, draws the exterior appearance figure of molecular sieve crystal；
Wherein, the step 2 includes：It is that point stacking forms dot matrix with selected primitive unit cell according to Dot Cellular Automata Mode Equation,
Obtain the mathematic(al) mode of crystal growing process Dynamic profiling.
2. the method for reproducing the crystallization process of molecular sieve according to claim 1 and describing its exterior appearance, which is characterized in that
The step 1 includes：
1) structural unit repeated in molecular sieve structure is analyzed, lists a variety of basic structure lists that may be present
Member；
2) analytical procedure 1) in basic structural unit, filter out that structural unit symmetry is high, follow-up Dot Cellular Automata form is succinct
Primitive unit cell of the basic structural unit as crystal growth.
3. the method for reproducing the crystallization process of molecular sieve according to claim 1 and describing its exterior appearance, which is characterized in that
The Dot Cellular Automata Mode Equation is deterministic type Dot Cellular Automata Mode Equation or probabilistic type Dot Cellular Automata Mode Equation.
4. the method for reproducing the crystallization process of molecular sieve according to claim 1 and describing its exterior appearance, which is characterized in that
The step 3 includes：
1) Numerical-Mode is carried out to crystal growth behavior using the serial/parallel row computational methods of multi-core computer to established mathematic(al) mode
It is quasi-；Molecular sieve average dimension is calculated in real time, molecular sieve is grown and carries out dynamic analog calcutation, and the position that calculating increases primitive unit cell newly is sat
Mark data；
2) acquired primitive unit cell space point data is updated, calculates the position data for obtaining molecular sieve crystal surface primitive unit cell.
5. the method for reproducing the crystallization process of molecular sieve according to claim 4 and describing its exterior appearance, which is characterized in that
In the serial/parallel row computational methods of multi-core computer, parallel computation number of unit is not less than 2.
6. the method for reproducing the crystallization process of molecular sieve according to claim 5 and describing its exterior appearance, which is characterized in that
The parallel computation number of unit is 4 computing units or more.
7. the method for reproducing the crystallization process of molecular sieve according to claim 1 and describing its exterior appearance, which is characterized in that
The step 4 includes：Surface interpolation is carried out to the position data of the surface primitive unit cell of acquisition, draws different moments, different resolution
Molecular sieve exterior appearance figure.
8. the method for reproducing the crystallization process of molecular sieve according to claim 7 and describing its exterior appearance, which is characterized in that
The surface interpolation uses spline surface mode.
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