CN101830482A - Preparation method of small crystal grain SAPO-34 molecular sieve - Google Patents
Preparation method of small crystal grain SAPO-34 molecular sieve Download PDFInfo
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- CN101830482A CN101830482A CN 201010199504 CN201010199504A CN101830482A CN 101830482 A CN101830482 A CN 101830482A CN 201010199504 CN201010199504 CN 201010199504 CN 201010199504 A CN201010199504 A CN 201010199504A CN 101830482 A CN101830482 A CN 101830482A
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Abstract
The invention discloses a preparation method of a small crystal grain SAPO-34 molecular sieve, which comprises the following steps of: 1. uniformly mixing pseudo boehmite and deionized water, sequentially adding orthophosphoric acid, alkali silica sol and triethylamine and uniformly mixing; 2. heating to the temperature of 90-180 DEG C, and stirring for 0.5-15 hours; 3. then heating to the temperature of 180-220 DEG C, and crystallizing for 24-72 hours in a static state and at constant temperature; and 4. cooling to room temperature, carrying out solid-liquid separation, washing a solid product to be neutral through the deionized water, drying and roasting to obtain the small crystal grain SAPO-34 molecular sieve. In the invention, the cheap triethylamine is used as a template agent, and before crystallization, a mixture obtained in step 1 is heated to certain temperature and stirred for a certain period of time, so that the synthesized molecular sieve has high crystallization degree, quite regular crystal forms, quite uniform grain diameter distribution with the average grain diameter of 2-3mu m and low synthetic cost and is hopeful to be used as a catalyst for preparing low-carbon olefine through methanol conversion.
Description
Technical field
The present invention relates to a kind of preparation method of fine grain SAPO-34 molecular sieve.
Background technology
U.S. Union Carbide Corp had developed a series of silicoaluminophosphamolecular molecular sieves in 1984, and what wherein people attracted attention the most is the SAPO-34 molecular sieve.This kind molecular sieve has small structure, medium tenacity is acid and good hydrothermal stability, this makes when it is applied to preparing low carbon olefinic hydrocarbon with methanol (MTO) reaction, the catalytic performance excellence, and methanol conversion reaches 100% or intimate 100%, the selectivity of ethene and propylene does not almost have C about 60%
5Above product.
European patent EP 0103117 and U.S. Pat 4440871 disclose the method for the synthetic SAPO-34 molecular sieve of a kind of hydro-thermal, use the mixture of tetraethyl ammonium hydroxide, Isopropylamine and tetraethyl ammonium hydroxide and dipropyl amine to be template in building-up process.But these template cost an arm and a leg, and are difficult in the industrial production and use.
U.S. Pat 5096684 discloses uses morpholine and HF as the method for the synthetic SAPO-34 molecular sieve of template, although do not re-use expensive tetraethyl ammonium hydroxide in this patent, because HF toxicity is bigger, also is not easy to industrial production and uses.European patent EP 2525160 discloses avoids highly toxic HF, and use can discharge the method for the compound of F-as the lower SAPO-34 molecular sieve of the synthetic silicone content of auxiliary template agent in system, but owing to the corrodibility of fluorochemical and the reason of price.Its application is restricted.
It is the method for the synthetic SAPO-34 molecular sieve of composite mould plate agent with the diethylamine that Chinese patent CN1096496 discloses a kind of, be template based on the diethylamine of cheapness or the organic compounds containing nitrogen of diethylamine in this patent, the synthetic catalyst cost reduces, but this method synthetic particle diameter is very big, one surpasses 15 μ m, cause catalyst life lower, selectivity of light olefin is also lower.
It is the method for the synthetic SAPO-34 molecular sieve of template with the triethylamine that Chinese patent CN1088483A discloses a kind of, be template with triethylamine or based on the nitrogenous organic mixture of triethylamine in this patent, under 100～225 ℃ of conditions, after the crystallization time is no less than 0.5 hour, after filtration, washing, drying obtain the SAPO-34 molecular sieve.This method uses cheap triethylamine to be template, has reduced the synthetic cost of SAPO-34 molecular sieve significantly, but the grain-size that obtains is bigger, and one is greater than 10 μ m.
Chinese patent CN101214974A discloses a kind of method for preparing fine grain SAPO-34 molecular sieve, also be that triethylamine with cheapness is a template in this patent, quickly synthesizing small-crystallite SAPO-34 molecular sieve under the ultrasonic wave aging condition, synthetic zeolite crystal size be decreased to traditional water thermal synthesis method preparation molecular sieve about 1/2nd.
In sum, can synthesize the less SAPO-34 molecular sieve of particle diameter, but this template is comparatively expensive, is unfavorable for industrial application by tetraethyl ammonium hydroxide; And when using cheap diethylamine or triethylamine as the synthetic SAPO-34 molecular sieve of template, institute's synthetic molecular sieve particle diameter is bigger, and when being used for preparing light olefins from methanol, selectivity of light olefin is lower, and the life-span of molecular sieve is shorter; Use cheap triethylamine to be template, can synthesize the SAPO-34 molecular sieve fast under the ultrasonic wave aging condition, particle diameter is little, but relatively difficulty is used in the aging skilled industry of ultrasonic wave.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of preparation method of fine grain SAPO-34 molecular sieve cheaply is provided.
Technical scheme of the present invention is summarized as follows:
A kind of preparation method of fine grain SAPO-34 molecular sieve, be made up of following steps:
(1), adds mass content successively and is 85% ortho-phosphoric acid, SiO with pseudo-boehmite and deionized water mixing
2Mass content is 15～40% alkaline silica sol, triethylamine mixing, makes the Al in the pseudo-boehmite
2O
3, the P suitable with ortho-phosphoric acid
2O
5, the SiO in the alkaline silica sol
2, triethylamine and H
2The mol ratio of O is: 1.0: 0.10～1.5: 0.2～0.8: 2.0～5.0: 30～70;
(2) be warming up to 90～180 ℃, stir 0.5～15h;
(3) be warming up to 180～220 ℃ again, static, thermostatic crystallization 24～72h;
(4) be cooled to room temperature, carry out solid-liquid separation, solid matter with deionized water is washed till neutrality, and after the drying, at 550 ℃, roasting 2-6h obtains fine grain SAPO-34 molecular sieve in air.
Step (2) is preferably: be warming up to 150 ℃, stir 1～8h.
Advantage of the present invention is:
The present invention uses cheap triethylamine to be template, by before crystallization, the mixture that step (1) is obtained is warming up to certain temperature, stir certain hour, make synthetic molecular sieve crystallinity height, crystal formation is very regular, median size is 2.5～5.5 μ m, only be 2.0～3.0 μ m after the optimal conditions, size distribution is very even, is expected to the catalyzer as methanol-to-olefins reaction.Synthetic cost is low.
Description of drawings
Fig. 1 is the XRD spectra of embodiment 1 synthetic fine grain SAPO-34 molecular sieve.
Fig. 2 is the stereoscan photograph of embodiment 1 synthetic fine grain SAPO-34 molecular sieve.
Fig. 3 is the XRD spectra of embodiment 2 synthetic fine grain SAPO-34 molecular sieves.
Fig. 4 is the stereoscan photograph of embodiment 2 synthetic fine grain SAPO-34 molecular sieves.
Fig. 5 is the stereoscan photograph of embodiment 3 synthetic fine grain SAPO-34 molecular sieves.
Fig. 6 is the stereoscan photograph of embodiment 4 synthetic fine grain SAPO-34 molecular sieves.
Fig. 7 is the stereoscan photograph of embodiment 5 synthetic fine grain SAPO-34 molecular sieves.
Embodiment
The present invention is further illustrated below in conjunction with specific embodiment.
Embodiment 1
The preparation method of Comparative Examples SAPO-34 molecular sieve, be made up of following steps:
(1) with 4g pseudo-boehmite (Al
2O
3Content is 65.4%) join in the 20.80g deionized water, after mixing, add the 5.91g mass content successively and be 85% ortho-phosphoric acid, 2.31g SiO
2Mass content is 40% alkaline silica sol, 7.77g triethylamine, mixes;
(2) mixture of step (1) acquisition is transferred in the crystallizing kettle, directly at 200 ℃ of thermostatic crystallization 48h;
(3) crystallization is cooled to room temperature with crystallizing kettle after finishing, and takes out the mother liquor centrifugation and obtains solid product, is washed till neutrality with deionized water, and at 120 ℃ of dry 12h, under 550 ℃, roasting obtained the SAPO-34 molecular sieve to remove template fully in 5 hours in the air again.
The XRD spectra of SAPO-34 molecular sieve and stereoscan photograph are seen Fig. 1 and Fig. 2 respectively.By XRD spectra as can be seen, present embodiment synthetic SAPO-34 molecular sieve purity is higher, does not contain stray crystal.Stereoscan photograph shows, synthetic SAPO-34 molecular sieve regular crystal forms, but size distribution is inhomogeneous, and particle size range is 2.0～10.0 μ m, and median size is 7 μ m.
Embodiment 2
A kind of preparation method of fine grain SAPO-34 molecular sieve is characterized in that being made up of following steps:
(1) with 4g pseudo-boehmite (Al
2O
3Content is 65.4%) join in the 20.80g deionized water, after mixing, add the 5.91g mass content successively and be 85% ortho-phosphoric acid, 2.31g SiO
2Mass content is 40% alkaline silica sol, 7.77g triethylamine, mixes;
(2) mixture of step (1) acquisition is transferred in the crystallizing kettle, is warming up to 150 ℃ and stirs 8h down;
(3) at 200 ℃ of thermostatic crystallization 48h;
(4) crystallization is cooled to room temperature with crystallizing kettle after finishing, and takes out the mother liquor centrifugation and obtains solid product, is washed till neutrality with deionized water, at 120 ℃ of dry 12h, under 550 ℃, roasting obtained fine grain SAPO-34 molecular sieve to remove template fully in 5 hours in the air again.
The XRD spectra and the stereoscan photograph of present embodiment synthetic fine grain SAPO-34 molecular sieve are seen Fig. 3 and Fig. 4 respectively.XRD spectra shows that synthetic SAPO-34 molecular sieve purity is higher, does not contain stray crystal.Stereoscan photograph shows that synthetic SAPO-34 molecular sieve crystal formation is very regular, and particle size distribution range is narrow, concentrates and is distributed in 2～3 μ m, and median size is 2.5 μ m.
Embodiment 3
A kind of preparation method of fine grain SAPO-34 molecular sieve is characterized in that being made up of following steps:
(1) with 4g pseudo-boehmite (Al
2O
3Content is 65.4%) join in the 20.80g deionized water, after mixing, add the 5.91g mass content successively and be 85% ortho-phosphoric acid, 2.31g SiO
2Mass content is 40% alkaline silica sol, 7.77g triethylamine, mixes;
(2) mixture of step (1) acquisition is transferred in the crystallizing kettle, is warming up to 90 ℃ and stirs 0.5h down;
(3) at 200 ℃ of thermostatic crystallization 72h;
(4) crystallization is cooled to room temperature with crystallizing kettle after finishing, and takes out the mother liquor centrifugation and obtains solid product, is washed till neutrality with deionized water, at 120 ℃ of dry 12h, under 550 ℃, roasting obtained fine grain SAPO-34 molecular sieve to remove template fully in 5 hours in the air again.
The stereoscan photograph of present embodiment synthetic SAPO-34 molecular sieve is seen Fig. 5.Stereoscan photograph shows that synthetic SAPO-34 molecular sieve crystal formation is very regular, and particle size range is 2.0～9.0 μ m, and median size is 5.5 μ m.
Embodiment 4
A kind of preparation method of fine grain SAPO-34 molecular sieve is characterized in that being made up of following steps:
(1) with 4g pseudo-boehmite (Al
2O
3Content is 65.4%) join in the 20.80g deionized water, after mixing, add the 5.91g mass content successively and be 85% ortho-phosphoric acid, 2.31g SiO
2Mass content is 40% alkaline silica sol, 7.77g triethylamine, mixes;
(2) mixture of step (1) acquisition is transferred in the crystallizing kettle, is warming up to 150 ℃ and stirs 15h down;
(3) at 220 ℃ of thermostatic crystallization 24h;
(4) crystallization is cooled to room temperature with crystallizing kettle after finishing, and takes out the mother liquor centrifugation and obtains solid product, is washed till neutrality with deionized water, at 120 ℃ of dry 12h, under 550 ℃, roasting obtained fine grain SAPO-34 molecular sieve to remove template fully in 6 hours in the air again.
The stereoscan photograph of present embodiment synthetic SAPO-34 molecular sieve is seen Fig. 6.Stereoscan photograph shows that synthetic SAPO-34 molecular sieve crystal formation is very regular, and particle size range is 3.0～8.0 μ m, and median size is 4.5 μ m.
A kind of preparation method of fine grain SAPO-34 molecular sieve is characterized in that being made up of following steps:
(1) with 4g pseudo-boehmite (Al
2O
3Content is 65.4%) join in the 20.80g deionized water, after mixing, add the 5.91g mass content successively and be 85% ortho-phosphoric acid, 2.31g SiO
2Mass content is 40% alkaline silica sol, 7.77g triethylamine, mixes;
(2) mixture of step (1) acquisition is transferred in the crystallizing kettle, is warming up to 180 ℃ and stirs 1h down;
(3) at 180 ℃ of thermostatic crystallization 48h;
(4) crystallization is cooled to room temperature with crystallizing kettle after finishing, and takes out the mother liquor centrifugation and obtains solid product, is washed till neutrality with deionized water, at 120 ℃ of dry 12h, under 550 ℃, roasting obtained fine grain SAPO-34 molecular sieve to remove template fully in 2 hours in the air again.
The XRD spectra and the stereoscan photograph of present embodiment synthetic SAPO-34 molecular sieve are seen Fig. 7 respectively.Stereoscan photograph shows that synthetic SAPO-34 molecular sieve crystal formation is very regular, and particle size range is 1.0～7.0 μ m, and median size is 2.5 μ m.
Embodiment 6
A kind of preparation method of fine grain SAPO-34 molecular sieve is characterized in that being made up of following steps:
(1) presses Al in the pseudo-boehmite
2O
3, the P suitable with ortho-phosphoric acid
2O
5, the SiO in the alkaline silica sol
2, triethylamine and H
2The mol ratio of O is: 1.0: 1.0: 0.5: 3.0: 50 with pseudo-boehmite (Al
2O
3Content is 65.4%) join in the deionized water, after mixing, add mass content successively and be 85% ortho-phosphoric acid, SiO
2Mass content is 40% alkaline silica sol, triethylamine, mixes;
Other step is with embodiment 2.
Embodiment 7
A kind of preparation method of fine grain SAPO-34 molecular sieve is characterized in that being made up of following steps:
(1) presses Al in the pseudo-boehmite
2O
3, the P suitable with ortho-phosphoric acid
2O
5, the SiO in the alkaline silica sol
2, triethylamine and H
2The mol ratio of O is: 1.0: 0.10: 0.2: 5.0: 70 with pseudo-boehmite (Al
2O
3Content is 65.4%) join in the deionized water, after mixing, add mass content successively and be 85% ortho-phosphoric acid, SiO
2Mass content is 40% alkaline silica sol, triethylamine, mixes;
Other step is with embodiment 2.
Embodiment 8
A kind of preparation method of fine grain SAPO-34 molecular sieve is characterized in that being made up of following steps:
(1) presses Al in the pseudo-boehmite
2O
3, the P suitable with ortho-phosphoric acid
2O
5, the SiO in the alkaline silica sol
2, triethylamine and H
2The mol ratio of O is: 1.0: 1.5: 0.8: 2.0: 30 with pseudo-boehmite (Al
2O
3Content is 65.4%) join in the deionized water, after mixing, add mass content successively and be 85% ortho-phosphoric acid, SiO
2Mass content is 40% alkaline silica sol, triethylamine, mixes;
Other step is with embodiment 2.
Experimental results show that embodiment 6-8 all can obtain regular crystal forms, median size is at 2.5～5.5 mu m ranges, and size distribution is fine grain SAPO-34 molecular sieve very uniformly.
From the spectrogram of the step of the preparation of above embodiment 1 and embodiment 2-8, product and photo relatively, the step of the preparation of embodiment 2-8 than embodiment more than 1 content of a step (2), this step reduces the median size of product just, and size distribution is very even.
Claims (2)
1. the preparation method of a fine grain SAPO-34 molecular sieve, be made up of following steps:
(1), adds mass content successively and is 85% ortho-phosphoric acid, SiO with pseudo-boehmite and deionized water mixing
2Mass content is 15～40% alkaline silica sol, triethylamine mixing;
(2) be warming up to 90～180 ℃, stir 0.5～15h;
(3) be warming up to 180～220 ℃ again, static, thermostatic crystallization 24～72h;
(4) be cooled to room temperature, carry out solid-liquid separation, solid matter with deionized water is washed till neutrality, and after the drying, at 550 ℃, roasting 2-6h obtains fine grain SAPO-34 molecular sieve in air.
2. the preparation method of a kind of fine grain SAPO-34 molecular sieve according to claim 1 is characterized in that described step (2) is: be warming up to 150 ℃, stir 1～8h.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102092737A (en) * | 2011-01-20 | 2011-06-15 | 南开大学 | Synthetic method of AlPO4-34 aluminum phosphate molecular sieve |
| CN102107885A (en) * | 2010-12-30 | 2011-06-29 | 天津凯美思特科技发展有限公司 | Preparation method of large-crystal-grain SAPO-34 molecular sieve |
| CN102336412A (en) * | 2011-06-24 | 2012-02-01 | 神华集团有限责任公司 | SAPO-34 molecular sieve preparation method |
| CN103408034A (en) * | 2013-06-22 | 2013-11-27 | 天津众智科技有限公司 | Preparation method of SAPO-34 molecular sieve with small average grain diameter |
| CN104229829A (en) * | 2013-06-17 | 2014-12-24 | 中国石油化工股份有限公司 | Preparation method of small grain SAPO-34 molecular sieve |
| CN104418358A (en) * | 2013-08-27 | 2015-03-18 | 中国科学院大连化学物理研究所 | Preparation method and application of small-crystal-grain SAPO-34 molecular sieve |
| CN105399109A (en) * | 2015-12-18 | 2016-03-16 | 西安元创化工科技股份有限公司 | Preparation method and applications of small crystalline grain silicoaluminophosphate molecular sieve |
| CN109761243A (en) * | 2019-02-21 | 2019-05-17 | 正大能源材料(大连)有限公司 | A kind of preparation of low silicon small grain SAPO-34 molecular sieve and application method |
| CN112624139A (en) * | 2019-09-24 | 2021-04-09 | 中国石油化工股份有限公司 | SAPO-34 molecular sieve and synthetic method and application thereof |
| CN115245838A (en) * | 2022-06-16 | 2022-10-28 | 天津大学 | T molecular sieve rapid synthesis method, catalyst and application |
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| CN1724161A (en) * | 2005-07-13 | 2006-01-25 | 清华大学 | Process for preparing load type silicon phoshporus aluminium molecular sieve |
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| CN1724161A (en) * | 2005-07-13 | 2006-01-25 | 清华大学 | Process for preparing load type silicon phoshporus aluminium molecular sieve |
| CN101214974A (en) * | 2007-12-29 | 2008-07-09 | 南开大学 | Method for preparing small crystal grain SAPO-34 molecular screen |
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102107885A (en) * | 2010-12-30 | 2011-06-29 | 天津凯美思特科技发展有限公司 | Preparation method of large-crystal-grain SAPO-34 molecular sieve |
| CN102092737A (en) * | 2011-01-20 | 2011-06-15 | 南开大学 | Synthetic method of AlPO4-34 aluminum phosphate molecular sieve |
| CN102092737B (en) * | 2011-01-20 | 2012-06-27 | 南开大学 | Synthetic method of AlPO4-34 aluminum phosphate molecular sieve |
| CN102336412A (en) * | 2011-06-24 | 2012-02-01 | 神华集团有限责任公司 | SAPO-34 molecular sieve preparation method |
| CN102336412B (en) * | 2011-06-24 | 2013-03-27 | 神华集团有限责任公司 | SAPO-34 molecular sieve preparation method |
| CN104229829B (en) * | 2013-06-17 | 2016-08-24 | 中国石油化工股份有限公司 | The method preparing fine grain SAPO-34 molecular sieve |
| CN104229829A (en) * | 2013-06-17 | 2014-12-24 | 中国石油化工股份有限公司 | Preparation method of small grain SAPO-34 molecular sieve |
| CN103408034B (en) * | 2013-06-22 | 2015-10-28 | 天津众智科技有限公司 | The preparation method of the SAPO-34 molecular sieve that median size is little |
| CN103408034A (en) * | 2013-06-22 | 2013-11-27 | 天津众智科技有限公司 | Preparation method of SAPO-34 molecular sieve with small average grain diameter |
| CN104418358A (en) * | 2013-08-27 | 2015-03-18 | 中国科学院大连化学物理研究所 | Preparation method and application of small-crystal-grain SAPO-34 molecular sieve |
| CN105399109A (en) * | 2015-12-18 | 2016-03-16 | 西安元创化工科技股份有限公司 | Preparation method and applications of small crystalline grain silicoaluminophosphate molecular sieve |
| CN105399109B (en) * | 2015-12-18 | 2018-06-12 | 西安元创化工科技股份有限公司 | A kind of preparation method and application of little crystal grain silicoaluminophosphamolecular molecular sieves |
| CN109761243A (en) * | 2019-02-21 | 2019-05-17 | 正大能源材料(大连)有限公司 | A kind of preparation of low silicon small grain SAPO-34 molecular sieve and application method |
| CN112624139A (en) * | 2019-09-24 | 2021-04-09 | 中国石油化工股份有限公司 | SAPO-34 molecular sieve and synthetic method and application thereof |
| CN112624139B (en) * | 2019-09-24 | 2022-11-04 | 中国石油化工股份有限公司 | SAPO-34 molecular sieve and synthetic method and application thereof |
| CN115245838A (en) * | 2022-06-16 | 2022-10-28 | 天津大学 | T molecular sieve rapid synthesis method, catalyst and application |
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