CN105738392A - Method for Measuring SAPO-11 Molecular Sieve Unit Cell Parameters - Google Patents
Method for Measuring SAPO-11 Molecular Sieve Unit Cell Parameters Download PDFInfo
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- CN105738392A CN105738392A CN201410766888.XA CN201410766888A CN105738392A CN 105738392 A CN105738392 A CN 105738392A CN 201410766888 A CN201410766888 A CN 201410766888A CN 105738392 A CN105738392 A CN 105738392A
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- sapo
- molecular sieve
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- cell parameter
- constant humidity
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- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical group [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 29
- 239000002808 molecular sieve Substances 0.000 claims abstract description 57
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000000634 powder X-ray diffraction Methods 0.000 claims abstract description 9
- 238000000227 grinding Methods 0.000 claims abstract description 6
- 239000010445 mica Substances 0.000 claims abstract description 4
- 229910052618 mica group Inorganic materials 0.000 claims abstract description 4
- 239000000843 powder Substances 0.000 claims abstract description 3
- 238000012937 correction Methods 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 9
- 230000004913 activation Effects 0.000 claims description 8
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 6
- 239000002250 absorbent Substances 0.000 claims description 5
- 230000002745 absorbent Effects 0.000 claims description 5
- 239000012047 saturated solution Substances 0.000 claims description 5
- 238000012360 testing method Methods 0.000 claims description 4
- QNRATNLHPGXHMA-XZHTYLCXSA-N (r)-(6-ethoxyquinolin-4-yl)-[(2s,4s,5r)-5-ethyl-1-azabicyclo[2.2.2]octan-2-yl]methanol;hydrochloride Chemical compound Cl.C([C@H]([C@H](C1)CC)C2)CN1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OCC)C=C21 QNRATNLHPGXHMA-XZHTYLCXSA-N 0.000 claims description 3
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 3
- 239000013078 crystal Substances 0.000 abstract description 5
- 238000002441 X-ray diffraction Methods 0.000 abstract description 4
- 230000003213 activating effect Effects 0.000 abstract 1
- 238000007873 sieving Methods 0.000 abstract 1
- 238000004458 analytical method Methods 0.000 description 7
- 238000005259 measurement Methods 0.000 description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical group [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- 229910025794 LaB6 Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000009499 grossing Methods 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 238000001144 powder X-ray diffraction data Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000012207 quantitative assay Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000010076 replication Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 238000012916 structural analysis Methods 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
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- Analysing Materials By The Use Of Radiation (AREA)
Abstract
A powder X-ray diffraction method for measuring SAPO-11 molecular sieve unit cell parameters comprises the following steps: (a) grinding, sieving, activating at high temperature, and absorbing water at constant humidity to obtain a sample to be tested; (b) respectively pressing a sample to be detected and a standard sample into corresponding sample holders of an X-ray diffractometer by taking NIST mica powder as the standard sample, respectively measuring the sample to be detected and the standard sample under the same working condition of the instrument, and collecting the measured X-ray diffraction data; (c) and (3) after correcting the diffraction angle by using NIST mica standard samples, calculating the unit cell parameters of the SAPO-11 molecular sieve according to an orthorhombic crystal face spacing formula.
Description
Technical field
The present invention relates to the method measuring SAPO-11 molecular sieve cell parameter, particularly relate to a kind of powder X-ray diffraction method measuring SAPO-11 molecular sieve cell parameter of employing.
Background technology
Molecular sieve is the crystal that a class has fixed space structure, and SAPO-11 molecular sieve, as wherein a member, is well applied in industry.In oil refining with chemical field, show the isomery performance of excellence.The space structure (such as the relative crystallinity of SAPO-11 molecular sieve, cell parameter etc.) that the quality of SAPO-11 molecular sieve isomery performance synthesizes with it has direct relation, generally effective assay method is to adopt powder X-ray diffractometry, but there is not been reported to adopt the method that the mensuration patent of SAPO-11 molecular sieve cell parameter, standard or research report are discussed in detail.Relate to SAPO-11 molecular sieve more be synthesis or the report of relevant catalyticing research, but generally also simply mention this mensuration with a few words simply wherein, do not describe concrete mensuration details.
It is the XRD determining that interior mark carries out SAPO-11 molecular sieve that document " synthesis of SAPO-11 configuration molecular sieve and X-ray diffraction structural analysis " describes employing KBr in August, 2000 at " Guizhou University's journal " the 17th volume 213-217 page, analysis process is not described.
nullDocument " X-ray diffraction method measure molecular sieve cell parameter and degree of crystallinity " in July, 2002 " physical and chemical inspection-physics fascicle " the 38th volume 298 pages by finely ground for NaY sample put to about 10 μm in an oven 110 DEG C be dried after，Then adopt and fill calcium chloride saturated solution constant humidity absorption 16 hours，Then for outer standard specimen, NaY sample after processing is carried out XRD determining with NaCl，Analyze cell parameter and degree of crystallinity，This kind of method is difficult in simple and easy method to realize finely ground for NaY to about 10 μm，The requirement of granularity is too harsh，Sieve needs special，Price is much more expensive，Additionally electrostatic problem is difficult to solve，Its drying means and standard sample is also had to be not appropriate for Accurate Determining SAPO-11 molecular sieve cell parameter，Simultaneously neither be best to the selection of constant humidity saturated solution.
The standard sample measuring molecular sieve has a variety of, such as silica flour, LaB6、Al2O3、SiO2Etc., other influence factor of standard specimen and the Accurate Determining SAPO-11 cell parameter demarcating SAPO-11 diffraction maximum can not be namely can determine that by limited experiment.
Summary of the invention
Based on problem above, present invention aim at providing a kind of quickly accurate, the simple method measuring SAPO-11 molecular sieve cell parameter.
The present invention provides a kind of powder X-ray diffraction method measuring SAPO-11 molecular sieve cell parameter, comprises the steps:
A () sample to be tested prepares
By sample through grinding, sieve, high-temperature activation, constant humidity water suction step, prepared sample to be tested；
B the mensuration of () X ray diffracting data is also collected
With NIST mica powder for standard specimen, sample to be tested is respectively pressed into standard specimen in corresponding X-ray diffractometer specimen holder, under identical instrument working condition, sample to be tested and standard specimen is measured respectively, and collects measured X ray diffracting data；
C (), with after the NIST Muscovitum standard specimen correction angle of diffraction, according to rhombic system interplanar distance formula, calculates the cell parameter of SAPO-11 molecular sieve.
Wherein, the peak position data of SAPO-11 molecular sieve sample (200), (020), (002) three crystallographic plane diffraction peak are corrected respectively with the peak position of 8.853 °, 17.759 °, 17.759 ° diffraction maximums of NIST Muscovitum standard specimen.
In step (a), testing sample is through grinding, and passing-screen size distribution is preferably 20 μm～50 μm, and maximum particle diameter and minimum grain size magnitude difference are preferably in less than 20 μm.
Maximum particle diameter and minimum grain size difference are preferably in less than 10 μm.
In step (a), high-temperature activation temperature is preferably 300 DEG C～400 DEG C, and soak time is preferably 2h～4h.
High-temperature activation temperature more preferably 350 DEG C in step (a), soak time is preferably 3h again.
Step (a) sample constant humidity absorbent time in the constant humidity cabinet filling magnesium chloride saturated solution is preferably 3～7 hours, and constant humidity water suction temperature is preferably 40 DEG C～60 DEG C.
In step (a), constant humidity water suction temperature is more preferably 50 DEG C, and constant humidity absorbent time is more preferably 5h.
The method have the advantages that offer is a kind of quickly and accurately, the simple method measuring SAPO-11 molecular sieve cell parameter, the present invention provides suitable SAPO-11 particle diameter test scope, avoid and cause diffraction peak intensity not high or diffraction peaks broadening phenomenon because granularity is bigger than normal or particle size distribution is wide in range in the process measuring SAPO-11 molecular sieve cell parameter, this particle size range is easily screened for simultaneously, not by too small for particle size range ceiling restriction, cause that electrostatic is difficult to eliminate, practical application is difficult to implement；Provide rational high-temperature activation temperature, it is ensured that remaining organic matter removal in molecular sieve, avoid that temperature is too high causes that framework shrinkage affects Accurate Determining cell parameter simultaneously；Provide constant humidity saturated solvent more preferably, adopt in constant humidity cabinet, properly increase constant humidity water suction temperature, substantially reduce constant humidity absorbent time.The outstanding feature of whole analysis process is time saving and energy saving.
Accompanying drawing explanation
Fig. 1 optimizes SAPO-11 molecular sieve X-ray diffraction curve after correction.
Detailed description of the invention
Set forth the present invention below in conjunction with embodiment, but be not limited to following example.
Embodiment 1
Adopting powder X-ray diffractometry to measure the cell parameter of SAPO-11 molecular sieve, sample producing process is as follows:
SAPO-11 molecular sieve is ground in agate mortar, it is 35.0 μm～45.0 μm that sample sifter after grinding separates the particle size distribution of granule, the sample screened out is positioned in the non-reactive crucible such as pottery, high-temperature activation 3h at 350 DEG C in Muffle furnace, it is reduced to after below 150 DEG C until muffle furnace, with crucible pliers, the non-reactive crucible such as pottery are transferred in the constant humidity cabinet filling magnesium chloride saturated solution in 50 DEG C of constant humidity water suction 5h, constant humidity water suction terminate after by sample load in specimen holder, adopt powder X-ray diffractometry measure SAPO-11 molecular sieve cell parameter.
Embodiment 2
Adopt powder x-ray diffraction that the analysis of SAPO-11 molecular sieve is measured to show: the diffracted intensity of diffraction maximum increases along with divergent slit, the increase receiving slit；Scanning step increases, and the point of a curve-distribution becomes dredges；Scanning speed is more slow, and curve is more smooth；Along with the increase of voltage, electric current, the diffracted intensity of product diffraction maximum is also linearly increasing.According to above-mentioned experiment, consider the factor such as intensity, the peak back of the body ratio, resolution, line smoothing degree, peak shape symmetry, it may be preferred to go out the best powder x-ray diffraction working condition of applicable SAPO-11 molecular sieve.
Table 1X x ray diffractometer x working condition
Embodiment 3
Carry out producing sample according to embodiment 1, sample to be tested and NIST Muscovitum standard specimen are respectively pressed in corresponding specimen holder, under the working condition of embodiment 2, carry out sample determination and collect powder X-ray diffraction data.Owing to SAPO-11 molecular sieve belongs to rhombic system, after the correction angle of diffraction, can according to interplanar distance formula: 1/d2=h2/a2+k2/b2+l2/c2, calculate the cell parameter of SAPO-11 molecular sieve.
The peak position data of SAPO-11 molecular sieve sample (200), (020), (002) three crystallographic plane diffraction peak are corrected respectively, such as Fig. 1 with the peak position of copper K α radiation 8.853 °, 17.759 °, the 17.759 ° diffraction maximums of angle of diffraction standard value of NIST Muscovitum standard specimen.
It is corrected seeing formula (1), (2), (3), (4), (5), (6) with the angular standard numerical value of NIST Muscovitum standard specimen diffraction maximum.
θ200 corrections=(2 θ200 actual measurements+8.853°-2θ8.853Mica surveys)/2………………………(1)
θ020 correction=(2 θ020 actual measurement+17.759°-2θ17.759Mica actual measurement)/2……………………(2)
θ002 correction=(2 θ002 actual measurement+17.759°-2θ17.759Mica actual measurement)/2……………………(3)
d200=λ/(2Sin θ200 corrections)…………………………………(4)
d020=λ/(2Sin θ020 correction)…………………………………(5)
d002=λ/(2Sin θ002 correction)…………………………………(6)
Note: λ copper KαX-ray wavelength (0.1542nm)
The cell parameter (a, b, c) of SAPO-11 molecular sieve calculates by formula (7), (8), (9) respectively, and numerical value represents with nm:
A=(d200 2×22)1/2…………………………………(7)
B=(d020 2×22)1/2…………………………………(8)
C=(d002 2×22)1/2…………………………………(9)
In formula:
The structure cell seamed edge a of a SAPO-11 molecular sieve；
The structure cell seamed edge b of b SAPO-11 molecular sieve；
The structure cell seamed edge c of c SAPO-11 molecular sieve；
d200The interplanar distance of SAPO-11 molecular sieve (200) crystal face；
d020The interplanar distance of SAPO-11 molecular sieve (020) crystal face；
d002The interplanar distance of SAPO-11 molecular sieve (002) crystal face；
Embodiment 4
Utilizing embodiment 1, embodiment 2, embodiment 3 method, SAPO-11 molecular sieve cell parameter has been measured at 12 laboratorys, the test data of gained is in Table 2, table 3 and table 4, and each sample replication twice, measurement result is accurate to after arithmetic point three.
The original analysis data (nm) of table 2SAPO-11 molecular sieve structure cell seamed edge c
The original analysis data (nm) of table 3SAPO-11 molecular sieve structure cell seamed edge b
The original analysis data (nm) of table 4SAPO-11 molecular sieve structure cell seamed edge a
Table 5SAPO-11 molecular sieve cell parameter collects (nm)
| a | 0.842 |
| b | 1.870 |
| c | 1.344 |
Optimized analysis measures SAPO-11 molecular sieve cell parameter a, b, c respectively 0.842nm, 1.870nm, 1.344nm.
Embodiment 5
By surveyed for this law SAPO-11 molecular sieve cell parameter value and International Molecular sieve association (InternationalZeoliteAssociation, IZA) SAPO-11 molecular sieve cell parameter value contrasts, both numerical value basically identical (see table 6), illustrate that this law measured value is accurate, reliable.
Table 6SAPO-11 molecular sieve cell parameter measured value contrast (nm)
| IZA | This law | |
| a | 0.831 | 0.842 |
| b | 1.873 | 1.870 |
| c | 1.339 | 1.344 |
The accurate cell parameter that the cell parameter that note: IZA announces is well recognized as.
The invention provides the quickly method of Accurate Determining SAPO-11 molecular sieve cell parameter, this kind of method is simple, convenient to carry out, simultaneously to have measurement result deviation little for the inventive method, the advantage that repeatability is high, it is applicable to qualitative quickly and accurately and/or quantitative assay SAPO-11 molecular sieve and cell parameter thereof, can be applicable in petrochemical iy produced industry.
Claims (8)
1. the powder X-ray diffraction method measuring SAPO-11 molecular sieve cell parameter, it is characterised in that:
A () sample to be tested prepares
By sample through grinding, sieve, high-temperature activation, constant humidity water suction step, prepared sample to be tested；
B the mensuration of () X ray diffracting data is also collected
With NIST mica powder for standard specimen, sample to be tested is respectively pressed into standard specimen in corresponding X-ray diffractometer specimen holder, under identical instrument working condition, sample to be tested and standard specimen is measured respectively, and collects measured X ray diffracting data；
C (), with after the NIST Muscovitum standard specimen correction angle of diffraction, according to rhombic system interplanar distance formula, calculates the cell parameter of SAPO-11 molecular sieve.
2. the method measuring SAPO-11 molecular sieve cell parameter described in claim 1, it is characterised in that: the peak position data of SAPO-11 molecular sieve sample (200), (020), (002) three crystallographic plane diffraction peak are corrected respectively with the peak position of 8.853 °, 17.759 °, 17.759 ° diffraction maximums of NIST Muscovitum standard specimen.
3. the method measuring SAPO-11 molecular sieve cell parameter described in claim 1, it is characterized in that: in step (a), testing sample is through grinding, passing-screen size distribution is 20 μm～50 μm, and maximum particle diameter and minimum grain size magnitude difference are below 20 μm.
4. the method measuring SAPO-11 molecular sieve cell parameter described in claim 3, it is characterised in that: maximum particle diameter and minimum grain size difference are below 10 μm.
5. the method measuring SAPO-11 molecular sieve cell parameter described in claim 1, it is characterised in that: in step (a), high-temperature activation temperature is 300 DEG C～400 DEG C, and soak time is 2h～4h.
6. the method measuring SAPO-11 molecular sieve cell parameter described in claim 5, it is characterised in that: high-temperature activation temperature preferably 350 DEG C in step (a), soak time is 3h.
7. the method measuring SAPO-11 molecular sieve cell parameter described in claim 1, its constant humidity water suction step (a) is characterised by: sample constant humidity absorbent time in the constant humidity cabinet filling magnesium chloride saturated solution is 3～7 hours, and constant humidity water suction temperature is 40 DEG C～60 DEG C.
8. the method measuring SAPO-11 molecular sieve cell parameter described in claim 7, it is characterised in that: in step (a), constant humidity water suction temperature is 50 DEG C, and constant humidity absorbent time is 5h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114380299A (en) * | 2020-10-22 | 2022-04-22 | 中国石油天然气股份有限公司 | SAPO-11 molecular sieve and synthetic method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4567029A (en) * | 1983-07-15 | 1986-01-28 | Union Carbide Corporation | Crystalline metal aluminophosphates |
| EP1350763A2 (en) * | 2001-01-05 | 2003-10-08 | China Petroleum & Chemical Corporation | Sapo-11 molecular sieve, its synthetic method and a catalyst containing the molecular sieve |
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2014
- 2014-12-11 CN CN201410766888.XA patent/CN105738392B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4567029A (en) * | 1983-07-15 | 1986-01-28 | Union Carbide Corporation | Crystalline metal aluminophosphates |
| EP1350763A2 (en) * | 2001-01-05 | 2003-10-08 | China Petroleum & Chemical Corporation | Sapo-11 molecular sieve, its synthetic method and a catalyst containing the molecular sieve |
Non-Patent Citations (3)
| Title |
|---|
| 储刚，陈刚: "X射线衍射法测定ZSM-5分子筛硅铝比", 《石油化工》 * |
| 胡启富: "SAPO-11构型分子筛的合成及X射线衍射结构分析", 《贵州大学学报（自然科学版）》 * |
| 马礼敦: "《近代X射线多晶体衍射-实验技术与数据分析》", 30 September 2004 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114380299A (en) * | 2020-10-22 | 2022-04-22 | 中国石油天然气股份有限公司 | SAPO-11 molecular sieve and synthetic method thereof |
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