CN102838127A - Primary crystallization hydrothermal preparation method of A-type and X-type molecular sieves containing pure Na ions - Google Patents
Primary crystallization hydrothermal preparation method of A-type and X-type molecular sieves containing pure Na ions Download PDFInfo
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- CN102838127A CN102838127A CN2012103704159A CN201210370415A CN102838127A CN 102838127 A CN102838127 A CN 102838127A CN 2012103704159 A CN2012103704159 A CN 2012103704159A CN 201210370415 A CN201210370415 A CN 201210370415A CN 102838127 A CN102838127 A CN 102838127A
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Abstract
The invention belongs to the technical field of microporous molecular sieve preparation, in particular to a primary crystallization hydrothermal preparation method of NaA and NaX microporous molecular sieves with adsorption cations which are all Na ions without a template agent, a guide agent and aging time. According to the preparation method, sodium aluminate (NaAlO2), sodium hydroxide (NaOH), sodium metasilicate nonahydrate (NA2SiO3.9H2O) and deionized water are used for synthesis, and two solutions based on a silicon source and an aluminum source are respectively prepared by synthetic steps; and the two solutions are uniformly stirred and then mixed, and after the mixed solution is persistently stirred for a period of time, the mixed solution is crystallized for several days in a high-temperature oven to obtain the NaA and NaX microporous molecular sieves with the adsorption cations which are all Na ions. The preparation method has the advantages of simple synthetic process, easiness of operation, convenience in industrialized production, commonality and easiness of obtaining reaction raw materials and low production cost, and the sizes of sample particles are 0.7-11 micrometers, so that the NaA and NaX microporous molecular sieves are moderate in sizes and convenient to use.
Description
Technical field
The invention belongs to the micro porous molecular sieve preparing technical field, the absorption positively charged ion that be specifically related to a kind ofly do not have template and directed agents, need not digestion time all is a crystallization hydrothermal preparing process of Na ionic NaA and NaX micro porous molecular sieve.
Background technology
As a kind of porous material; Micro porous molecular sieve (aperture is less than 2 nanometers) has extremely tempting performance; For example ion exchangeable, diffusion and adsorptivity, the shape property selected and catalytic activity and they can play an important role in the Subjective and Objective assembling chemical; This makes people to the demand of micro porous molecular sieve, and by the exploitation of the dependence natural zeolite that begins most (micro porous molecular sieve a kind of), it is synthetic mainly to rely on people's industry and commerce till now.By the end of 2006, the molecular sieve that international molecular sieve association is assert had about 170 kinds, wherein had only 17 kinds to carry out commercial syntheticly, and they are respectively AEL, AFY, BEA, CHA; EDI, FAU, FER, GIS, LTA, LTL; MER, MFI, MOR, MTT, MWW, TON and RHO type molecular sieve.
China and Cuba are the maximum countries of consumption of natural zeolite, and it is reported has about 2.4 hundred ten thousand tons zeolite molecular sieve mainly to be used for adding in the cement to increase cement intensity every year.In the U.S., Europe and Japanese, the consumption of natural zeolite has only 0.15 hundred ten thousand ton every year; Maximum commercial zeolite consumption is LTA type (4A; NaA) molecular sieve; This is main because the NaA molecular sieve is used to substitute tripoly phosphate sodium STPP (STPP) to be added in the washing powder as water-softening chemicals, and this has effectively been avoided the phosphatic excessive multiplication that excessively uses and discharge phycophyta in the rivers,lakes and seas of bringing.Though be not the use field of molecular sieve maximum, catalyzer market is the use field of synthesis of molecular sieve most worthy.Wherein synthetic FAU type zeolite molecular sieve accounts for 95% the share in catalyzer market.Oil refinery has been consumed most FAU type zeolite molecular sieves, is used for from crude oil, making gasoline (FCC facture).
At present, the synthetic technology of A type and X type micro porous molecular sieve has much at home.In CN 101172617A patent, the synthetic of A type molecular sieve need be at ultrasonic crystallization under the coldcondition.Though this method generated time is short, needs the part of low-temperature ultrasonic device as synthesis device.In CN 101337680A patent, it adopts directing agent method to synthesize the 4A zeolite molecular sieve.Though this method has shortened the crystallization time when synthetic and has obtained the product of small particle size, increased synthesis step and made building-up process complicated, also prolonged the generated time (the synthetic of directed agents needs 1～2 day) of product itself.In patent CN 1354132A, adopted the solvent pairs method to synthesize A type molecular sieve, wherein in the preparation process of microemulsion system, related to the accurate preparation of oil, tensio-active agent, the multiple material of cosurfactant, the more single solvent method of building-up process is complicated.And patent CN 100360405C has added the organism TMAH as template in the process of synthetic LTA (A) and FAU (X) type molecular sieve, and needs very long mixing the time (1～30 day), and experimental period is oversize.In the CN1724359A patent, it adopts crystal seed method to synthesize multiple molecular sieve, and this need add the substratum (raw material) of the required backbone element such as for example aluminium and silicon etc. of seeded growth in seed slurry; And to control the speed that substratum adds, speed with crystal growth is consistent basically to make it.Except the extra interpolation crystal seed of needs, this method also needs in the building-up process, and very accurate control techniques is arranged.Among the patent CN 101704534A, invented a kind of method based on the synthetic X type zeolite molecular sieve of Coaseries kaolin.Though this method has been used cheap reactant, building-up process comprised ageing 4～6 hours, crystallization 2～4 hours (60～80 ° of C) for the first time, and crystallization 12～48 hours (90～100 ° of C) for the second time, the process complicacy is time-consuming.
Summary of the invention
Synthetic present situation in view of present A type and X type micro porous molecular sieve; The invention provides and a kind ofly need not extra interpolation crystal seed, need not directed agents, need not template, do not need digestion time and do not need crystallization hydrothermal preparation A type of any organic additive and the method for X type molecular sieve, and the ion of absorption sun all is Na in the molecular sieve
+
The present invention uses sodium aluminate (NaAlO
2), sodium hydroxide (NaOH), nine water water glass (Na
2SiO
39H
2O) and deionized water (H
2O) synthesize; Synthesis step is to prepare two kinds of solution based on silicon source and aluminium source respectively; Mix after stirring, continue to stir after for some time in high temperature oven crystallization again and promptly got that to adsorb positively charged ion all be Na ionic NaA and NaX micro porous molecular sieve in several days.
Concrete synthesis step is following:
1. the preparation of silicon source solution
With 0.15～4.8 gram Na
2SiO
39H
2O joins in 10～15 ml deionized water, is stirred to dissolving evenly, obtains silicon source solution;
2. the preparation of aluminium source solution
(a) NaA type molecular sieve: with 0.15～1.5 gram NaAlO
2Join in 10～15 ml deionized water, be stirred to dissolving evenly, add 0.188～1.875 gram NaOH again and continue to stir 15～30 minutes, obtain aluminium source solution;
(b) NaX type molecular sieve: 0.3～1.2 gram NaOH is joined in 6.5～10 ml deionized water, be stirred to dissolving evenly, add 0.13～0.52 gram NaAlO again
2Continue to stir 15～30 minutes, obtain aluminium source solution;
3. crystallization
The aluminium source solution that will leave standstill then adds in the silicon source solution that is stirring slowly, continues to stir 30～50 minutes, and the reaction kettle of packing into then, crystallization is 1 hour～48 hours under 100 ℃ of conditions;
4. sample obtains and handles
After treating that crystallization is accomplished, cool off under the reaction kettle room temperature, then the white depositions in the solution is carried out the suction filtration oven dry, the powder that obtains white is NaA or NaX type molecular sieve.
Advantage of the present invention is that building-up process is simple, easy to operate, is convenient to industrialization production; Reaction raw materials is common, be prone to obtain, and production cost is low; The sample particle size is 0.7～11 micron.Be of moderate size convenient the use; The absorption positively charged ion all is Na
+, once synthetic.
Description of drawings
Fig. 1: the crystal particle diameter size is the scanning electron microscope diagram sheet (a) and the powder x-ray diffraction spectrogram (b) of 0.7 micron NaA type molecular sieve;
Fig. 2: the crystal particle diameter size is the scanning electron microscope diagram sheet (a) and the powder x-ray diffraction spectrogram (b) of 10 microns NaX type molecular sieve;
Fig. 3: the crystal particle diameter size is the scanning electron microscope diagram sheet of different amplification of 0.8 micron NaA type molecular sieve;
Fig. 4: the crystal particle diameter size is the scanning electron microscope diagram sheet of different amplification of 2 microns NaA type molecular sieve;
Fig. 5: the crystal particle diameter size is the scanning electron microscope diagram sheet of different amplification of 6.5 microns NaA type molecular sieve;
Fig. 6: the crystal particle diameter size is the scanning electron microscope diagram sheet of different amplification of 11 microns NaA type molecular sieve;
Fig. 7: the crystal particle diameter size is the scanning electron microscope diagram sheet of different amplification of 2 microns NaX type molecular sieve;
Fig. 8: the crystal particle diameter size is the scanning electron microscope diagram sheet of different amplification of 6 microns NaX type molecular sieve.
Among Fig. 1, scanning picture surface NaA type molecular sieve has good shapes and homogeneous particle diameter; Powder x-ray diffraction conforms to the standard spectrogram, shows that the crystal for preparing is the good NaA type molecular sieve of crystallization; The crystal grain size is about 0.7 micron;
Among Fig. 2, scanning picture surface NaX type molecular sieve has good shapes and homogeneous particle diameter; Powder x-ray diffraction conforms to the standard spectrogram, shows that the crystal for preparing is the good NaX type molecular sieve of crystallization; Crystallographic dimension is about 10 microns;
Can see among Fig. 3 that NaA type molecular sieve pattern is better, crystallization complete, the size homogeneous, size is 0.8 micron;
Can see among Fig. 4 that NaA type molecular sieve pattern is better, crystallization complete, the size homogeneous, size is 2 microns;
Can see among Fig. 5 that NaA type molecular sieve pattern is better, crystallization complete, the size homogeneous, size is 6.5 microns;
Can see among Fig. 6 that NaA type molecular sieve pattern is better, crystallization is complete, the size homogeneous, size is 11 microns;
Can see among Fig. 7 that NaX type molecular sieve pattern is better, crystallization is complete, the size homogeneous, size is 2 microns;
Can see among Fig. 8 that NaX type molecular sieve pattern is better, crystallization is complete, the size homogeneous, size is 6 microns.
Embodiment
Embodiment 1
The preparation of NaA type molecular sieve (0.7 micron):
With 1.5 gram NaAlO
2Join in 10 ml deionized water, after stirring makes its uniform dissolution, add 1.875 gram NaOH and continue to stir 30 minutes, leave standstill for a moment; Obtain aluminium source solution.
With 1.5 gram Na
2SiO
39H
2O joins in 10 ml deionized water, and stirring and dissolving obtains silicon source solution until evenly.
The aluminium source solution that will leave standstill then adds in the silicon source solution that is stirring slowly, continues to stir 30 minutes, and the teflon-lined stainless steel cauldron of packing into, crystallization is 5 hours under 100 ℃ of conditions, and the suction filtration oven dry obtains NaA type molecular sieve (0.7 micron).The gained sample size is even, crystallization good (accompanying drawing 1), and productive rate 70～75%, Si/Al=1:1, the aperture is 0.4nm.
Embodiment 2
The preparation of NaX type molecular sieve (10 microns):
0.3 gram NaOH is joined in 6.5 ml deionized water, after stirring, add 0.13 gram NaAlO
2Continue to stir 30 minutes, leave standstill a moment; Obtain aluminium source solution.
With 1.2 gram Na
2SiO
39H
2O joins in 15 ml deionized water, stirs until evenly, obtains silicon source solution.
In the silicon source solution that the aluminium source slow adding of solution that will leave standstill is then being stirred, continue to stir the teflon-lined stainless steel cauldron of packing into 30 minutes; Crystallization is 3 days under 100 ℃ of conditions; The suction filtration oven dry obtains NaX type molecular sieve powder (10 microns) (accompanying drawing 2), productive rate 70～75%; Si/Al=1:1.3, the aperture is 1.0nm.
Embodiment 3
The preparation of NaA type molecular sieve (0.8 micron):
With 0.75 gram NaAlO
2Join in 10 ml deionized water, after stirring makes its uniform dissolution, add 0.94 gram NaOH and continue to stir 30 minutes, leave standstill for a moment; Obtain aluminium source solution.
With 0.75 gram Na
2SiO
39H
2O joins in 10 ml deionized water, and stirring and dissolving obtains silicon source solution until evenly.
The aluminium source solution that will leave standstill then adds in the silicon source solution that is stirring slowly, continues to stir 30 minutes, and the teflon-lined stainless steel cauldron of packing into, crystallization is 1 hour under 100 ℃ of conditions, and the suction filtration oven dry obtains NaA type molecular sieve (0.8 micron).The gained sample size is even, crystallization good (accompanying drawing 3), and productive rate 70～75%, Si/Al=1:1, the aperture is 0.4nm.
Embodiment 4
The preparation of NaA type molecular sieve (2 microns):
With 0.5 gram NaAlO
2Join in 10 ml deionized water, after stirring makes its uniform dissolution, add 0.63 gram NaOH and continue to stir 30 minutes, leave standstill for a moment; Obtain aluminium source solution.
With 0.5 gram Na
2SiO
39H
2O joins in 10 ml deionized water, and stirring and dissolving obtains silicon source solution until evenly.
The aluminium source solution that will leave standstill then adds in the silicon source solution that is stirring slowly, continues to stir 50 minutes, and the teflon-lined stainless steel cauldron of packing into, crystallization is 1 hour under 100 ℃ of conditions, and the suction filtration oven dry obtains NaA type molecular sieve (2 microns).The gained sample size is even, crystallization good (accompanying drawing 4), and productive rate 70～75%, Si/Al=1:1, the aperture is 0.4nm.
Embodiment 5
The preparation of NaA type molecular sieve (6.5 microns):
With 0.3 gram NaAlO
2Join in 10 ml deionized water, after stirring makes its uniform dissolution, add 0.37 gram NaOH and continue to stir 30 minutes, leave standstill for a moment; Obtain aluminium source solution.
With 0.3 gram Na
2SiO
39H
2O joins in 10 ml deionized water, and stirring and dissolving obtains silicon source solution until evenly.
The aluminium source solution that will leave standstill then adds in the silicon source solution that is stirring slowly, continues to stir 30 minutes, and the teflon-lined stainless steel cauldron of packing into, crystallization is 3 hours under 100 ℃ of conditions, and the suction filtration oven dry obtains NaA type molecular sieve (6.5 microns).The gained sample size is even, crystallization good (accompanying drawing 5), and productive rate 70～75%, Si/Al=1:1, the aperture is 0.4nm.
Embodiment 6
The preparation of NaA type molecular sieve (11 microns):
With 0.15 gram NaAlO
2Join in 10 ml deionized water, after stirring makes its uniform dissolution, add 0.188 gram NaOH and continue to stir 30 minutes, leave standstill for a moment; Obtain aluminium source solution.
With 0.15 gram Na
2SiO
39H
2O joins in 10 ml deionized water, and stirring and dissolving obtains silicon source solution until evenly.
The aluminium source solution that will leave standstill then adds in the silicon source solution that is stirring slowly, continues to stir 30 minutes, and the teflon-lined stainless steel cauldron of packing into, crystallization is 3 hours under 100 ℃ of conditions, and the suction filtration oven dry obtains NaA type molecular sieve (11 microns).The gained sample size is even, crystallization good (accompanying drawing 6), and productive rate 70～75%, Si/Al=1:1, the aperture is 0.4nm.
Embodiment 7
The preparation of NaX type molecular sieve (6 microns):
0.6 gram NaOH is joined in 6.5 ml deionized water, after stirring makes its uniform dissolution, add 0.26 gram NaAlO
2Continue to stir 30 minutes, leave standstill a moment; Obtain aluminium source solution.
With 2.4 gram Na
2SiO
39H
2O joins in 15 ml deionized water, stirs until evenly, obtains silicon source solution.
In the silicon source solution that the aluminium source slow adding of solution that will leave standstill is then being stirred, continue to stir the teflon-lined stainless steel cauldron of packing into 30 minutes; Crystallization is 2 days under 100 ℃ of conditions; The suction filtration oven dry obtains NaX type molecular sieve powder (6 microns) (accompanying drawing 7), productive rate 70～75%; Si/Al=1:1.3, the aperture is 1.0nm.
Embodiment 8
The preparation of NaX type molecular sieve (2 microns):
With 1.2 gram NaOH join stir in 6.5 ml deionized water after, add 0.52 gram NaAlO
2Continue to stir 30 minutes, leave standstill a moment; Obtain aluminium source solution.
With 4.8 gram Na
2SiO
39H
2O joins in 15 ml deionized water and stirs until evenly, obtains silicon source solution.
In the silicon source solution that the aluminium source slow adding of solution that will leave standstill is then being stirred, continue to stir the teflon-lined stainless steel cauldron of packing into 50 minutes; Crystallization is 1 day under 100 ℃ of conditions; The suction filtration oven dry obtains NaX type molecular sieve powder (2 microns) (accompanying drawing 8), productive rate 70～75%; Si/Al=1:1.3, the aperture is 1.0nm.
Claims (2)
1. contain a crystallization hydrothermal preparing process of pure Na ionic A type molecular sieve, its step is following:
1) preparation of silicon source solution
With 0.15～4.8 gram Na
2SiO
39H
2O adds in 10～15 ml deionized water, is stirred to dissolving evenly, obtains silicon source solution;
2) preparation of aluminium source solution
With 0.15～1.5 gram NaAlO
2Add in 10～15 ml deionized water, be stirred to dissolving evenly, add 0.188～1.875 gram NaOH again and continue to stir 15～30 minutes, obtain aluminium source solution;
3) crystallization
The aluminium source solution that leaves standstill is added in the silicon source solution that is stirring slowly, continue to stir 30～50 minutes, the reaction kettle of packing into then, crystallization is 1 hour～48 hours under 100 ℃ of conditions;
4) sample obtains and handles
After treating that crystallization is accomplished, cool off under the reaction kettle room temperature, with the oven dry of the white depositions suction filtration in the solution, the powder that obtains white is and contains pure Na ionic A type molecular sieve then.
2. contain a crystallization hydrothermal preparing process of pure Na ionic X type molecular sieve, its step is following:
1) preparation of silicon source solution
With 0.15～4.8 gram Na
2SiO
39H
2O adds in 10～15 ml deionized water, is stirred to dissolving evenly, obtains silicon source solution;
2) preparation of aluminium source solution
0.3～1.2 gram NaOH is added in 6.5～10 ml deionized water, be stirred to dissolving evenly, add 0.13～0.52 gram NaAlO again
2Continue to stir 15～30 minutes, obtain aluminium source solution;
3) crystallization
The aluminium source solution that leaves standstill is added in the silicon source solution that is stirring slowly, continue to stir 30～50 minutes, the reaction kettle of packing into then, crystallization is 1 hour～48 hours under 100 ℃ of conditions;
4) sample obtains and handles
After treating that crystallization is accomplished, cool off under the reaction kettle room temperature, with the oven dry of the white depositions suction filtration in the solution, the powder that obtains white is and contains pure Na ionic X type molecular sieve then.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103435062A (en) * | 2013-08-20 | 2013-12-11 | 昆明理工大学 | Rapid preparation method for A-type nano zeolite molecular sieve |
| CN104528763A (en) * | 2014-12-17 | 2015-04-22 | 上海大学 | Preparation method of X-type zeolite molecular sieve |
| CN104591208A (en) * | 2015-01-16 | 2015-05-06 | 中国地质大学（武汉） | X-type zeolite having FAU frame structure and preparation method thereof |
| CN105195029A (en) * | 2015-10-21 | 2015-12-30 | 吉林大学 | Method for synthesizing NaA type molecular sieve crystals and synthesizing NaA type molecular sieve film |
| CN105600802A (en) * | 2015-12-30 | 2016-05-25 | 山西大同大学 | Preparation method of silicon-aluminum microporous molecular sieve |
| CN107512728A (en) * | 2017-07-03 | 2017-12-26 | 深圳大学 | The preparation method of card plugging structure multi-stage porous FAU type zeolite molecular sieves |
| CN110498423A (en) * | 2019-09-20 | 2019-11-26 | 苏州立昂新材料有限公司 | A kind of preparation method of nano type A molecular sieve |
| CN112744827A (en) * | 2021-01-05 | 2021-05-04 | 江南大学 | Method for synthesizing ferrierite molecular sieve by seed crystal method |
| CN112939012A (en) * | 2021-04-16 | 2021-06-11 | 许昌学院 | Nano X-type zeolite and rapid preparation method thereof |
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| US20050090380A1 (en) * | 2003-10-27 | 2005-04-28 | Council Of Scientific And Industrial Research | Process for the preparation of molecular sieve adsorbent for selective adsorption of oxygen from air |
| CN1721325A (en) * | 2004-07-12 | 2006-01-18 | 中国石油化工股份有限公司 | Process for preparing fine grain zeolite |
| CN102417190A (en) * | 2011-09-02 | 2012-04-18 | 吉林大学 | Method for preparing low-silicon NaX zeolite by applying activated silicon source |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103435062A (en) * | 2013-08-20 | 2013-12-11 | 昆明理工大学 | Rapid preparation method for A-type nano zeolite molecular sieve |
| CN104528763A (en) * | 2014-12-17 | 2015-04-22 | 上海大学 | Preparation method of X-type zeolite molecular sieve |
| CN104591208A (en) * | 2015-01-16 | 2015-05-06 | 中国地质大学（武汉） | X-type zeolite having FAU frame structure and preparation method thereof |
| CN105195029A (en) * | 2015-10-21 | 2015-12-30 | 吉林大学 | Method for synthesizing NaA type molecular sieve crystals and synthesizing NaA type molecular sieve film |
| CN105600802A (en) * | 2015-12-30 | 2016-05-25 | 山西大同大学 | Preparation method of silicon-aluminum microporous molecular sieve |
| CN107512728A (en) * | 2017-07-03 | 2017-12-26 | 深圳大学 | The preparation method of card plugging structure multi-stage porous FAU type zeolite molecular sieves |
| CN107512728B (en) * | 2017-07-03 | 2020-06-26 | 深圳大学 | Preparation method of FAU type zeolite molecular sieve with card-inserted structure and hierarchical pores |
| CN110498423A (en) * | 2019-09-20 | 2019-11-26 | 苏州立昂新材料有限公司 | A kind of preparation method of nano type A molecular sieve |
| CN112744827A (en) * | 2021-01-05 | 2021-05-04 | 江南大学 | Method for synthesizing ferrierite molecular sieve by seed crystal method |
| CN112939012A (en) * | 2021-04-16 | 2021-06-11 | 许昌学院 | Nano X-type zeolite and rapid preparation method thereof |
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Application publication date: 20121226 |