CN102992350A - SAPO-31 molecular sieve and preparation method thereof - Google Patents
SAPO-31 molecular sieve and preparation method thereof Download PDFInfo
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Abstract
An SAPO-31 molecular sieve and a preparation method thereof relate to a molecular sieve and a preparation method thereof. The invention aims to solve problems in an existing preparation method of the SAPO-31 molecular sieve, such as long crystallization time, low yield, complex operation, unsuitability for mass production, high cost of the prepared SAPO-31, and easy generation of SAPO-5 mixed crystal, SAPO-11 mixed crystal and SiO2 mixed crystal. The SAPO-31molecular sieve is prepared from phosphoric acid, pseudoboehmite, silica sol and di-n-butylamine. The preparation method comprises steps of: 1. initial gel preparation; 2. crystallization; and 3. roasting to obtain the SAP-O31 molecular sieve. The invention is applicable to the fields of catalyst and petrochemical processing.
Description
Technical field
The present invention relates to SAPO-31 molecular sieve and preparation method thereof.
Background technology
Aluminosilicophosphate SAPO-31 molecular sieve (ATO type topological framework with twelve-ring one-dimensional tunnel structure, pore size is 0.54 * 0.54nm), because the effect of contraction in its duct, be conducive to the generation of the less single branched chain isomer of molecular dynamics size, make the generation of the relatively large two side chains of molecular dynamics size or highly-branched chain isomerous body limited.Because but the SAPO-31 molecular sieve has suitable pore passage structure size, the acidity of gentleness modulation, so supporting the dual-function catalyst of precious metal/base metal preparation as acid carrier, the SAPO-31 molecular sieve in long carbochain normal paraffin hygrogenating isomerization reaction, shows preferably catalytic activity and isomerization selectivity.
Adopting costliness and the poor aluminum isopropylate of safety in utilization among the preparation method of SAPO-31 molecular sieve at present is the aluminium source, adopting the higher silicon aerosol of price is that silicon source and the di-n-propylamine that easily guides multiple crystalline phase to form are template, it is long to prepare the required crystallization time of SAPO-31 molecular sieve, yield is lower, complicated operation, can not carry out scale operation, there is the cost height in the SAPO-31 molecular sieve for preparing and is prone to SAPO-5 stray crystal, SAPO-11 stray crystal and SiO
2The problem of stray crystal.
Summary of the invention
The present invention will solve to have among the preparation method of existing SAPO-31 molecular sieve that crystallization time is long, yield is lower, complicated operation, can not carry out scale operation, and the SAPO-31 for preparing exists cost high and be prone to SAPO-5 stray crystal, SAPO-11 stray crystal and SiO
2The problem of stray crystal, and provide a kind of SAPO-31 molecular sieve new preparation method.
A kind of SAPO-31 molecular sieve is to be prepared from by phosphoric acid, pseudo-boehmite, silicon sol and Di-n-Butyl Amine; Wherein, the mass ratio of pseudo-boehmite and phosphoric acid is (0.40 ~ 0.70): 1, and the mass ratio of silicon sol and phosphoric acid is (0.30 ~ 0.90): 1, the mass ratio of Di-n-Butyl Amine and phosphoric acid is (0.50 ~ 0.90): 1.
A kind of preparation method of SAPO-31 molecular sieve, specifically finish according to the following steps:
One, add pseudo-boehmite, silicon sol, Di-n-Butyl Amine and water in phosphoric acid, the stir speed (S.S.) stirring 5h ~ 7h at 800r/min ~ 1000r/min obtains initial gel; Wherein, the mass ratio of pseudo-boehmite and phosphoric acid is (0.40 ~ 0.70): 1, and the mass ratio of silicon sol and phosphoric acid is (0.30 ~ 0.90): 1, the mass ratio of Di-n-Butyl Amine and phosphoric acid is (0.50 ~ 0.90): 1, the mass ratio of water and phosphoric acid is (2.0 ~ 4.0): 1;
Two, the initial gel that step 1 is obtained joins in the crystallizing kettle, crystallization 2h ~ 48h under 170 ℃ ~ 190 ℃ temperature, be cooled to 20 ℃ ~ 25 ℃, obtain solidliquid mixture, with the solidliquid mixture that obtains dry 10h ~ 24h after centrifugal, washing, under 100 ℃ ~ 120 ℃ temperature, obtain solid;
Three, the solid that step 2 is obtained, under 500 ℃ ~ 700 ℃ temperature, constant temperature calcining 6h ~ 8h naturally cools to 20 ℃ ~ 30 ℃, has namely obtained the SAPO-31 molecular sieve.
Advantage of the present invention: one, a kind of SAPO-31 molecular sieve provided by the invention and preparation method thereof, adopt cheap pseudo-boehmite and silicon sol to be respectively aluminium source and silicon source, adopting cheap Di-n-Butyl Amine is template, not only cost is low for the SAPO-31 molecular sieve for preparing, and because the employing Di-n-Butyl Amine is template, the SAPO-31 molecular sieve that is synthesized is not prone to SAPO-5, SAPO-11 and SiO
2Stray crystal; Two, a kind of SAPO-31 molecular sieve provided by the invention and preparation method thereof, preparation process is simple, and easy handling, yield more than 85%, are fit to large-scale industrialization production than Gao Keda; Three, a kind of SAPO-31 molecular sieve provided by the invention and preparation method thereof can prepare the SAPO-31 molecular sieve of wider silica alumina ratio scope, makes the SAPO-31 molecular sieve have wider acid density and strength of acid variable range.
Description of drawings
Fig. 1 is the X-ray diffractogram of the test one SAPO-31 molecular sieve for preparing.
Fig. 2 is the scanning electron microscope diagram of the test one SAPO-31 molecular sieve for preparing.
Fig. 3 is the X-ray diffractogram of the test two SAPO-31 molecular sieves that prepare.
Fig. 4 is the scanning electron microscope diagram of the test two SAPO-31 molecular sieves that prepare.
Fig. 5 is the X-ray diffractogram of the test three SAPO-31 molecular sieves that prepare.
Fig. 6 is the scanning electron microscope diagram of the test three SAPO-31 molecular sieves that prepare.
Fig. 7 is the X-ray diffractogram of the test four SAPO-31 molecular sieves that prepare.
Fig. 8 is the scanning electron microscope diagram of the test four SAPO-31 molecular sieves that prepare.
Embodiment
Embodiment one: present embodiment provides a kind of SAPO-31 molecular sieve, is prepared from by phosphoric acid, pseudo-boehmite, silicon sol and Di-n-Butyl Amine; Wherein, the mass ratio of pseudo-boehmite and phosphoric acid is (0.40 ~ 0.70): 1, and the mass ratio of silicon sol and phosphoric acid is (0.30 ~ 0.90): 1, the mass ratio of Di-n-Butyl Amine and phosphoric acid is (0.50 ~ 0.90): 1.
Present embodiment has the following advantages: one, the SAPO-31 molecular sieve that provides of present embodiment, adopt cheap pseudo-boehmite and silicon sol to be respectively aluminium source and silicon source, adopting cheap Di-n-Butyl Amine is template, not only cost is low for the SAPO-31 molecular sieve for preparing, and because the employing Di-n-Butyl Amine is template, the SAPO-31 molecular sieve that is synthesized is not prone to SAPO-5, SAPO-11 and SiO
2Stray crystal; Two, the SAPO-31 molecular sieve that provides of present embodiment has wider silica alumina ratio scope, makes the SAPO-31 molecular sieve have wider acid density and strength of acid variable range.
Embodiment two: the difference of present embodiment and embodiment one is that the mass percent concentration of described phosphoric acid is 85%.Other is identical with embodiment one.
Embodiment three: present embodiment is the method for preparing embodiment one described a kind of SAPO-31 molecular sieve, specifically finishes according to the following steps:
One, add pseudo-boehmite, silicon sol, Di-n-Butyl Amine and water in phosphoric acid, the stir speed (S.S.) stirring 5h ~ 7h at 800r/min ~ 1000r/min obtains initial gel; Wherein, the mass ratio of pseudo-boehmite and phosphoric acid is (0.40 ~ 0.70): 1, and the mass ratio of silicon sol and phosphoric acid is (0.30 ~ 0.90): 1, the mass ratio of Di-n-Butyl Amine and phosphoric acid is (0.50 ~ 0.90): 1, the mass ratio of water and phosphoric acid is (2.0 ~ 4.0): 1;
Two, the initial gel that step 1 is obtained joins in the crystallizing kettle, crystallization 2h ~ 48h under 170 ℃ ~ 190 ℃ temperature, be cooled to 20 ℃ ~ 25 ℃, obtain solidliquid mixture, with the solidliquid mixture that obtains dry 10h ~ 24h after centrifugal, washing, under 100 ℃ ~ 120 ℃ temperature, obtain solid;
Three, the solid that step 2 is obtained, under 500 ℃ ~ 700 ℃ temperature, constant temperature calcining 6h ~ 8h naturally cools to 20 ℃ ~ 30 ℃, has namely obtained the SAPO-31 molecular sieve.
Present embodiment has the following advantages: one, a kind of SAPO-31 molecular sieve of providing of present embodiment and preparation method thereof, adopt cheap pseudo-boehmite and silicon sol to be respectively aluminium source and silicon source, adopting cheap Di-n-Butyl Amine is template, not only cost is low for the SAPO-31 molecular sieve for preparing, and because the employing Di-n-Butyl Amine is template, the SAPO-31 molecular sieve that is synthesized is not prone to SAPO-5, SAPO-11 and SiO
2Stray crystal; Two, a kind of SAPO-31 molecular sieve of providing of present embodiment and preparation method thereof, preparation process is simple, and easy handling, yield more than 90%, are fit to large-scale industrialization production than Gao Keda; Three, a kind of SAPO-31 molecular sieve of providing of present embodiment and preparation method thereof can prepare the SAPO-31 molecular sieve of wider silica alumina ratio scope, makes the SAPO-31 molecular sieve have wider acid density and strength of acid variable range.
Embodiment four: the difference of present embodiment and embodiment three is that the mass percent concentration of the phosphoric acid of described step 1 is 85%.Other is identical with embodiment three.
Embodiment five: present embodiment and embodiment three or fours' difference is that the water of described step 1 is deionized water.Other is identical with embodiment three or four.
Embodiment six: the difference of one of present embodiment and embodiment three to five is that the stir speed (S.S.) of described step 1 is 1000r/min, and churning time is 6h.Other is identical with one of embodiment three to five.
Embodiment seven: the difference of one of present embodiment and embodiment three to six is that the condition of the crystallization of described step 2 is crystallization 2h under 180 ℃ temperature.Other is identical with embodiment three to six.
Embodiment eight: the difference of one of present embodiment and embodiment three to seven is that the condition of the crystallization of described step 2 is crystallization 20h under 180 ℃ temperature.Other is identical with embodiment three to seven.
Embodiment nine: the difference of one of present embodiment and embodiment three to eight is that the drying mode of described step 2 is dry 12h under 110 ℃ temperature.Other is identical with embodiment three to eight.
Embodiment ten: the difference of one of present embodiment and embodiment three to nine is that the condition of the constant temperature calcining of described step 3 is constant temperature calcining 6h under 600 ℃ temperature.Other is identical with embodiment three to nine.
Adopt following verification experimental verification effect of the present invention:
Test one: a kind of preparation method of SAPO-31 molecular sieve, specifically finish according to the following steps:
One, add pseudo-boehmite, silicon sol, Di-n-Butyl Amine and water in phosphoric acid, the stir speed (S.S.) stirring 6h at 1000r/min obtains initial gel; Wherein, the mass ratio of pseudo-boehmite and phosphoric acid is 0.6:1, and the mass ratio of silicon sol and phosphoric acid is 0.6:1, and the mass ratio of Di-n-Butyl Amine and phosphoric acid is 0.8:1, and the mass ratio of water and phosphoric acid is 3:1;
Two, the initial gel that step 1 is obtained joins in the crystallizing kettle, and crystallization 2h under 180 ℃ temperature is cooled to 25 ℃, obtains solidliquid mixture, and after centrifugal, washing, dry 12h obtains solid under 110 ℃ temperature with the solidliquid mixture that obtains;
Three, the solid that step 2 is obtained, constant temperature calcining 6h under 600 ℃ temperature naturally cools to 25 ℃, has namely obtained the SAPO-31 molecular sieve.Its yield can reach 79.3%.
Carry out the X-ray diffraction test to testing a SAPO-31 molecular sieve for preparing, obtain Fig. 1.From Fig. 1, can observe at 2 θ is 8.5 °, 20.2 °, 22.0 ° and 22.5 ° of characteristic diffraction peaks of locating all to have the SAPO-31 molecular sieve, and without other stray crystal.
Carry out scanning electron microscope test to testing a SAPO-31 molecular sieve for preparing, obtain Fig. 2.From Fig. 2, can observe the SAPO-31 molecular sieve is bar-like grains.
Test two: a kind of preparation method of SAPO-31 molecular sieve, specifically finish according to the following steps:
One, add pseudo-boehmite, silicon sol, Di-n-Butyl Amine and water in phosphoric acid, the stir speed (S.S.) stirring 6h at 1000r/min obtains initial gel; Wherein, the mass ratio of pseudo-boehmite and phosphoric acid is 0.6:1, and the mass ratio of silicon sol and phosphoric acid is 0.6:1, and the mass ratio of Di-n-Butyl Amine and phosphoric acid is 0.8:1, and the mass ratio of water and phosphoric acid is 3:1;
Two, the initial gel that step 1 is obtained joins in the crystallizing kettle, and crystallization 20h under 180 ℃ temperature is cooled to 25 ℃, obtains solidliquid mixture, and after centrifugal, washing, dry 12h obtains solid under 110 ℃ temperature with the solidliquid mixture that obtains;
Three, the solid that step 2 is obtained, constant temperature calcining 6h under 600 ℃ temperature naturally cools to 25 ℃, has namely obtained the SAPO-31 molecular sieve.Its yield can reach 85.1%.
Carry out the X-ray diffraction test to testing the two SAPO-31 molecular sieves that prepare, obtain Fig. 3.From Fig. 3, can observe at 2 θ is 8.5 °, 20.2 °, 22.0 ° and 22.5 ° of characteristic diffraction peaks of locating all to have the SAPO-31 molecular sieve, and without other stray crystal.
Carry out scanning electron microscope test to testing the two SAPO-31 molecular sieves that prepare, obtain Fig. 4.From Fig. 4, can observe the SAPO-31 molecular sieve is bar-like grains.
Test three: a kind of preparation method of SAPO-31 molecular sieve, specifically finish according to the following steps:
One, add pseudo-boehmite, silicon sol, Di-n-Butyl Amine and water in phosphoric acid, the stir speed (S.S.) stirring 6h at 1000r/min obtains initial gel; Wherein, the mass ratio of pseudo-boehmite and phosphoric acid is 0.6:1, and the mass ratio of silicon sol and phosphoric acid is 0.5:1, and the mass ratio of Di-n-Butyl Amine and phosphoric acid is 0.8:1, and the mass ratio of water and phosphoric acid is 3:1;
Two, the initial gel that step 1 is obtained joins in the crystallizing kettle, and crystallization 24h under 180 ℃ temperature is cooled to 25 ℃, obtains solidliquid mixture, with the solidliquid mixture that obtains dry 12h after centrifugal, washing, under 110 ℃ temperature, obtains solid;
Three, the solid that step 2 is obtained, under 600 ℃ temperature, constant temperature calcining 6h naturally cools to 25 ℃, has namely obtained the SAPO-31 molecular sieve.Its yield can reach 88.7%.
Carry out the X-ray diffraction test to testing the three SAPO-31 molecular sieves that prepare, obtain Fig. 5.From Fig. 5, can observe at 2 θ is 8.5 °, 20.2 °, 22.0 ° and 22.5 ° of characteristic diffraction peaks of locating all to have the SAPO-31 molecular sieve, and without other stray crystal.
Carry out scanning electron microscope test to testing the three SAPO-31 molecular sieves that prepare, obtain Fig. 6.From Fig. 6, can observe the SAPO-31 molecular sieve is bar-like grains.
Test four: a kind of preparation method of SAPO-31 molecular sieve, specifically finish according to the following steps:
One, add pseudo-boehmite, silicon sol, Di-n-Butyl Amine and water in phosphoric acid, the stir speed (S.S.) stirring 6h at 1000r/min obtains initial gel; Wherein, the mass ratio of pseudo-boehmite and phosphoric acid is 0.6:1, and the mass ratio of silicon sol and phosphoric acid is 0.8:1, and the mass ratio of Di-n-Butyl Amine and phosphoric acid is 0.8:1, and the mass ratio of water and phosphoric acid is 3:1;
Two, the initial gel that step 1 is obtained joins in the crystallizing kettle, and crystallization 24h under 180 ℃ temperature is cooled to 25 ℃, obtains solidliquid mixture, with the solidliquid mixture that obtains dry 12h after centrifugal, washing, under 110 ℃ temperature, obtains solid;
Three, the solid that step 2 is obtained, constant temperature calcining 6h under 600 ℃ temperature naturally cools to 25 ℃, has namely obtained the SAPO-31 molecular sieve.Its yield can reach 89.1%.
Carry out the X-ray diffraction test to testing the four SAPO-31 molecular sieves that prepare, obtain Fig. 7.From Fig. 7, can observe at 2 θ is 8.5 °, 20.2 °, 22.0 ° and 22.5 ° of characteristic diffraction peaks of locating all to have the SAPO-31 molecular sieve, and without other stray crystal.
Carry out scanning electron microscope test to testing a SAPO-31 molecular sieve for preparing, obtain Fig. 8.From Fig. 8, can observe the SAPO-31 molecular sieve is bar-like grains.
Claims (10)
1. SAPO-31 molecular sieve, it is characterized in that: the SAPO-31 molecular sieve is to be prepared from by phosphoric acid, pseudo-boehmite, silicon sol and Di-n-Butyl Amine; Wherein, the mass ratio of pseudo-boehmite and phosphoric acid is (0.40 ~ 0.70): 1, and the mass ratio of silicon sol and phosphoric acid is (0.30 ~ 0.90): 1, the mass ratio of Di-n-Butyl Amine and phosphoric acid is (0.50 ~ 0.90): 1.
2. a kind of SAPO-31 molecular sieve according to claim 1, it is characterized in that: the mass percent concentration of described phosphoric acid is 85%.
3. the preparation method of a kind of SAPO-31 molecular sieve as claimed in claim 1, it is characterized in that: the preparation method specifically finishes according to the following steps:
One, add pseudo-boehmite, silicon sol, Di-n-Butyl Amine and water in phosphoric acid, the stir speed (S.S.) stirring 5h ~ 7h at 800r/min ~ 1000r/min obtains initial gel; Wherein, the mass ratio of pseudo-boehmite and phosphoric acid is (0.40 ~ 0.70): 1, and the mass ratio of silicon sol and phosphoric acid is (0.30 ~ 0.90): 1, the mass ratio of Di-n-Butyl Amine and phosphoric acid is (0.50 ~ 0.90): 1, the mass ratio of water and phosphoric acid is (2.0 ~ 4.0): 1;
Two, the initial gel that step 1 is obtained joins in the crystallizing kettle, crystallization 2h ~ 48h under 170 ℃ ~ 190 ℃ temperature, be cooled to 20 ℃ ~ 25 ℃, obtain solidliquid mixture, with the solidliquid mixture that obtains after centrifugal, washing, dry 10h ~ 24h under 100 ℃ ~ 120 ℃ temperature obtains solid;
Three, the solid that step 2 is obtained under 500 ℃ ~ 700 ℃ temperature, behind constant temperature calcining 6h ~ 8h, naturally cools to 20 ℃ ~ 30 ℃, has namely obtained the SAPO-31 molecular sieve.
4. the preparation method of a kind of SAPO-31 molecular sieve according to claim 3, it is characterized in that: the mass percent concentration of the phosphoric acid of described step 1 is 85%.
5. according to claim 3 or the preparation method of 4 described a kind of SAPO-31 molecular sieves, it is characterized in that: the water of described step 1 is deionized water.
6. according to claim 3 or the preparation method of 4 described a kind of SAPO-31 molecular sieves, it is characterized in that: the stir speed (S.S.) of described step 1 is 1000r/min, and churning time is 6h.
7. the preparation method of a kind of SAPO-31 molecular sieve according to claim 3 is characterized in that: the condition of the crystallization of described step 2 is crystallization 2h under 180 ℃ temperature.
8. according to claim 3, the preparation method of 4 or 7 described a kind of SAPO-31 molecular sieves, it is characterized in that: the condition of the crystallization of described step 2 is crystallization 20h under 180 ℃ temperature.
9. according to claim 3, the preparation method of 4 or 7 described a kind of SAPO-31 molecular sieves, it is characterized in that: the drying mode of described step 2 is dry 12h under 110 ℃ temperature.
10. according to claim 3, the preparation method of 4 or 7 described a kind of SAPO-31 molecular sieves, it is characterized in that: the roasting condition of described step 3 is at 600 ℃ roasting temperature 6h.
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| CN103482647A (en) * | 2013-10-15 | 2014-01-01 | 黑龙江大学 | Synthetic method of MgSAPO-31 molecular sieve |
| CN103553077A (en) * | 2013-11-13 | 2014-02-05 | 黑龙江大学 | Synthetic method of SAPO-31 molecular sieve with hierarchical pores |
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| CN102275949A (en) * | 2011-07-14 | 2011-12-14 | 黑龙江大学 | Preparation method of nano SAPO-31 molecular sieve |
| CN102424399A (en) * | 2011-09-05 | 2012-04-25 | 中国科学院过程工程研究所 | Preparation process for aluminosilicophosphate molecular sieve |
| CN102807229A (en) * | 2012-08-10 | 2012-12-05 | 中国海洋石油总公司 | Method for synthesizing SAPO-31 (silicoaluminophosphate-31) molecular sieves at ordinary pressure |
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| CN102275949A (en) * | 2011-07-14 | 2011-12-14 | 黑龙江大学 | Preparation method of nano SAPO-31 molecular sieve |
| CN102424399A (en) * | 2011-09-05 | 2012-04-25 | 中国科学院过程工程研究所 | Preparation process for aluminosilicophosphate molecular sieve |
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| CN103553077B (en) * | 2013-11-13 | 2015-08-19 | 黑龙江大学 | A kind of synthetic method with the SAPO-31 molecular sieve of multi-stage porous |
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