CN103274427A - Preparation method for P-shaped molecular sieve - Google Patents
Preparation method for P-shaped molecular sieve Download PDFInfo
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- CN103274427A CN103274427A CN2013102403360A CN201310240336A CN103274427A CN 103274427 A CN103274427 A CN 103274427A CN 2013102403360 A CN2013102403360 A CN 2013102403360A CN 201310240336 A CN201310240336 A CN 201310240336A CN 103274427 A CN103274427 A CN 103274427A
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Abstract
The invention discloses a preparation method for a P-shaped molecular sieve, which comprises the following steps: firstly, uniformly mixing a silicon source, an aluminium source, sodium hydroxide and water to form a precursor, then adding certain amount of silicon-alumininm molecular sieves with GIS structures to be taken as seed crystals, crystallizing for 4 to 168 hours at the temperature of 70 to 190 DEG C, washing and drying the crystallized solid product, and gaining the P-shaped molecular sieve. Through the adoption of the method that the silicon source and the aluminium source with higher activity are taken as raw materials; and the seed crystals are added, the gelatinous silicon-alumininm can be enabled to surround the seed crystal to grow rapidly; the single kettle productive rate of the prepared P-shaped molecular sieve is enabled to be high; the particle size distribution of the crystal is uniform; the relative crystallinity is higher; and the molecular sieve can be used for adsorbing cations in water, and can also be used for adsorbing and separating water vapour in gas.
Description
Technical field
The present invention relates to contain in the skeleton preparation method of the molecular sieve with GIS structure of silicon, aluminium element, be specifically related to a kind of preparation method of P type molecular sieve.
Background technology
P type molecular sieve is a kind of zeolite molecular sieve that early synthesizes, and has the GIS structure in octatomic ring intersection duct, and its scantlings of the structure is respectively
With
Its unique pore structure provides the space constraint effect for the selection adsorptivity of gas, simultaneously because the cationic existence of balancing charge makes the effective pore radius of P type molecular sieve exist
About, except H
2O, NH
3Deng the less gas of kinetic diameter, do not adsorb other components, in addition, P type molecular sieve is to Ca in the aqueous solution
2+, Mg
2+Plasma has selectivity preferably, and these characteristics make P type molecular sieve in fields such as washing auxiliary detergent, water treatment and fractionation by adsorption comparatively wide application be arranged.
Naturally occurring garranite (garronite), amicite (amicite), dagger-axe silicon sodium aluminium stone (gobbinsite) and gismondite (also claim gismondine, gismondine), because mineral products are few, the exploitation difficulty is big, and purity is low, and the composition complexity is not generally made such use.
Document The crystal structure of synthetic zeolite Na-P1, reported a kind of synthetic method (Baerlocher of P type molecular sieve among an isotype of gismondine (isomorphous thing of the crystalline structure of synthetic molecular sieve Na-P1---gismondite), C., Meier, W.M.Z.Kristallogr. (1972) .135,339-354.).This method uses water glass and sodium metaaluminate as raw material, at 100～120 ℃, reacts and obtains P type molecular sieve after 3 days.
Document Structure of a high-silica variety of zeolite Na-P. (a kind of Na-P molecular sieve of high silicon content synthetic) reported a kind of high silicon P type molecular sieve synthetic method (Acta Cryst. (1990) .C46,1363-1364.).This method is the silicon source with the soda glass,, is transferred in the crystallization container after mixing by a certain percentage as alkali source with NaOH, at 200 ℃, reacts and obtains high silicon P type molecular sieve after 7 days.
US Patent No. 3008803A has reported a kind of synthetic method of P type molecular sieve, and this method is the silicon source with the hydrated SiO 2, is the aluminium source with the aluminum oxide, after sodium hydroxide mixes by a certain percentage, behind 100 ℃ of reaction 71h, obtains P type molecular sieve.
Chinese patent application prospectus CN1769172A has reported a kind of fast synthesis method of P type molecular sieve, this method is used and is contained the sodium aluminate solution of water glass as raw material, add crystal seed, utilize the mechanochemical reaction reaction to make P type molecular sieve, this method has been used industrial intermediate raw material, cost is relatively low, and has added crystal seed, and resultant velocity is fast.
The synthetic method of reporting in existing literature and the patent, under the situation of not adding crystal seed, because long reaction time, the inefficiency of preparation is not suitable for industry's enlarging production.Though and the CN1769172A reported method has himself advantage because the raw silicon aluminum ratio that uses easy-regulating not, and contain more impurity, and use the synthetic molecular sieve of mechanochemical reaction on degree of crystallinity and degree of uniformity all not as hydrothermal synthesis method.
Summary of the invention
The objective of the invention is the deficiency at above P type molecular sieve synthetic method, provide a kind of step simple, and can synthesize the preparation method of P type molecular sieve fast.
The fast preparation method of P type molecular sieve provided by the present invention may further comprise the steps:
1) silicon source, aluminium source, sodium hydroxide and water are mixed the formation presoma, wherein the amount of each raw material is pressed the silicon source with SiO
2Meter, the aluminium source is with Al
2O
3Meter, sodium hydroxide is with Na
2O meter, the mol ratio of they and water is Al
2O
3: SiO
2: Na
2O: H
2O=1: 2～5: 3～7: 50～250;
2) Si-Al molecular sieve with a certain amount of GIS of having structure adds in the above-mentioned presoma equably as crystal seed, and the add-on of crystal seed is with contained Al wherein
2O
3The amount of substance meter, be Al in the presoma
2O
3The 2-50% (mol ratio) of amount of substance, crystallization 4h～168h under 70～190 ℃ of temperature then, and with the washing of crystallization gained solid product, oven dry, obtain P type molecular sieve.
The method according to this invention, the source of silicon described in the step 1) can be selected from one or more in white carbon black, silicon sol, water glass and the organosilicon acid esters, is preferably water glass
Wherein, to be generally carbonatoms be 1～4 organosilicon acid esters to described organosilicon acid esters.Further, described carbonatoms is that 1～4 organosilicon acid esters is preferably methyl silicate and/or tetraethyl silicate.
The method according to this invention, the source of aluminium described in the step 1) can be selected from one or more in aluminum oxide, hydrated aluminum oxide, aluminum soluble salt, aluminate and the organic pure aluminum compound.Wherein, described hydrated aluminum oxide includes but not limited to one or more in gibbsite, boehmite, pseudo-boehmite and the surge aluminium stone etc.; Described aluminum soluble salt includes but not limited to one or more in aluminum chloride, aluminum nitrate, the Tai-Ace S 150 etc.; Described aluminate includes but not limited to one or more in sodium metaaluminate, the potassium metaaluminate etc.; It is 1～4 organic pure aluminum compound that described organic pure aluminum compound is selected carbonatoms usually, more preferably aluminum isopropylate.Further, described aluminium source is preferably one or more in Tai-Ace S 150, aluminum nitrate, aluminum chloride and the sodium metaaluminate, wherein more preferably sodium metaaluminate.
Further, the method according to this invention, step 2) Si-Al molecular sieve with GIS structure as crystal seed described in can be synthetic P type molecular sieve, also can be that natural molecule sieve mineral such as garranite (garronite), amicite (amicite), dagger-axe silicon sodium aluminium stone (gobbinsite) and the gismondite with GIS structure (also claims gismondine, gismondine) in one or more.Wherein, the described Si-Al molecular sieve with GIS structure as crystal seed is preferably the P type molecular sieve of synthetic.
The method according to this invention, in the step 1), preferred presoma consists of: Al
2O
3: SiO
2: Na
2O: H
2O=1: 2～5: 4～6: 80～220 (mol ratios).
The method according to this invention, step 2) in, crystallization temperature is preferably 90～150 ℃, and crystallization time is preferably 4h～24h.
The method according to this invention, step 2) crystallization process in can be crystallization process known in the field.This crystallization process both can be the dynamic crystallization process, also can be the static crystallization process, preferred dynamic crystallization process.
The method according to this invention, step 2) be conventionally known to one of skill in the art to the product washing that obtains after the crystallization, dry method, after for example adopting the washing repeatedly of water and alcohol solvent, dry more than 12 hours under temperature is 100 ℃, obtain P type molecular sieve product.Wherein, the consumption of cleaning solvent can be selected according to concrete reaction during washing, generally speaking, can be 1-10 times of reaction volume.
The present invention carries by selecting for use active higher silicon source (as water glass) and aluminium source (as sodium metaaluminate) as raw material, add the method for crystal seed again, make the sial of gel can center on seeded growth rapidly, make prepared P type molecular sieve single-autoclave yield rate height, crystal particle diameter is evenly distributed, relative crystallinity is higher, and it can be used for positively charged ion in the planar water, also can be used for the water vapor of adsorption seperation of gas.
Description of drawings
Fig. 1 is the X-ray diffractogram of the P type molecular sieve P1 that obtains among the embodiment 1.
Fig. 2 is the electron scanning micrograph of the P type molecular sieve P1 that obtains among the embodiment 1.
Embodiment
Below the present invention will be described in detail by specific embodiment, but the present invention is not restricted to following embodiment.
In following examples, the mean grain size of measuring zeolite adopts Scherrer (Scherrer) equation (seeing that " commercial catalysts analytical test illness that has not attacked the vital organs of the human body " Liu Xiyao etc. writes, hydrocarbon processing press, nineteen ninety publication) to measure by x-ray powder diffraction (XRD); The relative crystallinity of zeolite is standard by the product that xrd method synthesizes with document " The crystal structure of synthetic zeolite Na-P1, an isotype of gismondine " reported method.
In following examples, water glass is available from Qingdao Dongyue Sodium Silicate Co., Ltd., and all the other reagent are all available from the Beijing Chemical Plant.
Embodiment 1
Present embodiment is used for the fast preparation method of explanation P type molecular sieve.
With water glass, sodium metaaluminate, sodium hydroxide and water according to Al
2O
3: SiO
2: Na
2O: H
2O=1: the mixed of 5: 5: 180 (mol ratio) evenly back forms presoma, adds a certain amount of P type molecular sieve crystal seed, wherein Al
2O
3Amount of substance account for Al in the whole presoma
2O
35% of molar weight, dynamic crystallization 24h under 100 ℃ of temperature took out washing, 100 ℃ of dryings after 12 hours, obtained product P 1.Measure the relative crystallinity of this product P 1, list in table 1.The XRD spectra of P1 is referring to Fig. 1, and the electron scanning micrograph of P1 is referring to Fig. 2.XRD figure by Fig. 1 as can be known, P1 is P type molecular sieve.
Present embodiment is used for the fast preparation method of explanation P type molecular sieve.
With silicon sol, Tai-Ace S 150, sodium hydroxide and water according to Al
2O
3: SiO
2: Na
2O: H
2O=1: the mixed of 4: 3: 100 (mol ratio) evenly back forms presoma, adds a certain amount of P type molecular sieve crystal seed, wherein Al
2O
3Amount of substance account for Al in the whole presoma
2O
315% of molar weight, dynamic crystallization 18h under 120 ℃ of temperature took out washing, 100 ℃ of dryings after 12 hours, obtained product P 2.Measure the relative crystallinity of this product P 2, list in table 1.XRD figure by P2 as can be known, P2 is P type molecular sieve.
Embodiment 3
Present embodiment is used for the fast preparation method of explanation P type molecular sieve.
With water glass, aluminum nitrate, sodium hydroxide and water according to Al
2O
3: SiO
2: Na
2O: H
2O=1: the mixed of 3.7: 4: 120 (mol ratio) evenly back forms presoma, adds a certain amount of P type molecular sieve crystal seed, wherein Al
2O
3Amount of substance account for Al in the whole presoma
2O
310% of molar weight, dynamic crystallization 24h under 110 ℃ of temperature took out washing, 100 ℃ of dryings after 12 hours, obtained product P 3.Measure the relative crystallinity of this product P 3, list in table 1.XRD figure by P3 as can be known, P3 is P type molecular sieve.
Embodiment 4
Present embodiment is used for the fast preparation method of explanation P type molecular sieve.
With white carbon black, sodium metaaluminate, sodium hydroxide and water according to A1
2O
3: SiO
2: Na
2O: H
2O=1: the mixed of 3.5: 4.5: 150 (mol ratio) evenly back forms presoma, adds a certain amount of P type molecular sieve crystal seed, wherein Al
2O
3Amount of substance account for Al in the whole presoma
2O
310% of molar weight, dynamic crystallization 18h under 120 ℃ of temperature took out washing, 100 ℃ of dryings after 12 hours, obtained product P 4.Measure the relative crystallinity of this product P 4, list in table 1.XRD figure by P4 as can be known, P4 is P type molecular sieve.
Embodiment 5
Present embodiment is used for the fast preparation method of explanation P type molecular sieve.
With water glass, aluminum chloride, sodium hydroxide and water according to Al
2O
3: SiO
2: Na
2O: H
2O=1: the mixed of 3: 5: 180 (mol ratio) evenly back forms presoma, adds a certain amount of P type molecular sieve crystal seed, wherein Al
2O
3Amount of substance account for Al in the whole presoma
2O
315% of molar weight, dynamic crystallization 12h under 150 ℃ of temperature took out washing, 100 ℃ of dryings after 12 hours, obtained product P 5.Measure the relative crystallinity of this product P 5, list in table 1.XRD figure by P5 as can be known, P5 is P type molecular sieve.
Comparative Examples 1
According to document The crystal structure of synthetic zeolite Na-P1, the synthetic method of the P type molecular sieve of reporting among an isotype of gismondine.Concrete steps are as follows:
With water glass, sodium metaaluminate, sodium hydroxide and water, according to Al
2O
3: SiO
2: Na
2O: H
2O=1: 3.7: 2.2: 70 (mol ratio), at 100 ℃, react and obtain P type molecular sieve after 3 days and be designated as D1.Measure the relative crystallinity of this sample, the results are shown in table 1.XRD spectra by D1 as can be known, D1 is P type molecular sieve.
Table 1
| ? | Comparative Examples 1 | Embodiment 1 | |
Embodiment 3 | Embodiment 4 | Embodiment 5 |
| Relative crystallinity (%) | 99.7 | 113.1 | 107.2 | 99.6 | 105.2 | 102.9 |
| Single-autoclave yield rate (weight %) | 78.2 | 92.1 | 93.8 | 91.2 | 90.3 | 94.1 |
By table 1 as can be known, adopt the P type molecular sieve relative crystallinity of method preparation provided by the invention significantly higher, and generated time is shorter, in addition, adopts method provided by the invention, makes single-autoclave yield rate improve 12-16 percentage point.
Claims (10)
1. the preparation method of a P type molecular sieve comprises the steps:
1) silicon source, aluminium source, sodium hydroxide and water are mixed the formation presoma, wherein the amount of each raw material is pressed the silicon source with SiO
2Meter, the aluminium source is with Al
2O
3Meter, sodium hydroxide is with Na
2O meter, the mol ratio of they and water is Al
2O
3: SiO
2: Na
2O: H
2O=1: 2～5: 3～7: 50～250;
2) Si-Al molecular sieve of a certain amount of GIS of having structure is added in the presoma that step 1) forms equably as crystal seed, the add-on of crystal seed is with contained Al wherein
2O
3The amount of substance meter be Al in the presoma
2O
3The 2-50% of amount of substance, crystallization 4h～168h under 70～190 ℃ of temperature then, and with the washing of crystallization gained solid product, oven dry, obtain P type molecular sieve.
2. preparation method as claimed in claim 1 is characterized in that, the source of silicon described in the step 1) is selected from one or more in white carbon black, silicon sol, water glass and the organosilicon acid esters.
3. preparation method as claimed in claim 2 is characterized in that, described organosilicon acid esters is that carbonatoms is 1～4 organosilicon acid esters.
4. preparation method as claimed in claim 1 is characterized in that, the source of aluminium described in the step 1) is selected from one or more in aluminum oxide, hydrated aluminum oxide, aluminum soluble salt, aluminate and the organic pure aluminum compound.
5. preparation method as claimed in claim 4 is characterized in that, described hydrated aluminum oxide is selected from one or more in gibbsite, boehmite, pseudo-boehmite and the surge aluminium stone; Described aluminum soluble salt is selected from one or more in aluminum chloride, aluminum nitrate, the Tai-Ace S 150; Described aluminate is sodium metaaluminate and/or potassium metaaluminate; Described organic pure aluminum compound is that carbonatoms is 1～4 organic pure aluminum compound.
6. preparation method as claimed in claim 1, it is characterized in that, step 2) Si-Al molecular sieve with GIS structure as crystal seed described in is synthetic P type molecular sieve and/or the sieve of the natural molecule with GIS structure mineral, and the natural molecule sieve mineral of the wherein said GIS of having structure are selected from one or more in garranite, amicite, dagger-axe silicon sodium aluminium stone and the gismondite.
7. preparation method as claimed in claim 1 is characterized in that, each component of presoma is in molar ratio in the step 1): Al
2O
3: SiO
2: Na
2O: H
2O=1: 2～5: 4～6: 80～220.
8. preparation method as claimed in claim 1 is characterized in that step 2) in the temperature of crystallization process be 90～150 ℃, the time is 4h～24h.
9. preparation method as claimed in claim 1 is characterized in that step 2) the crystallization mode is static crystallization or dynamic crystallization.
10. preparation method as claimed in claim 1 is characterized in that step 2) crystallization gained solid product adopts water and alcohol solvent to wash, then 100 ℃ dry more than 12 hours down, obtain P type molecular sieve.
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|---|---|---|---|---|
| CN103787356A (en) * | 2014-01-24 | 2014-05-14 | 东南大学 | Preparation method for hierarchical pore P-type molecular sieve |
| CN104528755A (en) * | 2014-12-26 | 2015-04-22 | 上海大学 | Method for preparing P1-type molecular sieve |
| CN104591202A (en) * | 2013-11-04 | 2015-05-06 | 中国石油化工股份有限公司 | Hollow P type zeolite and preparation method thereof |
| CN106745058A (en) * | 2016-12-28 | 2017-05-31 | 河南大学 | A kind of microwave preparation of p-type molecular sieve |
| CN107381524A (en) * | 2017-08-15 | 2017-11-24 | 中国神华能源股份有限公司 | The method and NaP molecular sieves of NaP molecular sieves are prepared using white clay as raw material |
| CN108246239A (en) * | 2018-02-12 | 2018-07-06 | 东北石油大学 | The method of metal-doped KP types adsorbent of molecular sieve removing carbonyl sulfur |
| WO2018218736A1 (en) * | 2017-06-02 | 2018-12-06 | 中山大学 | Aluminosilicate zeolite molecular sieve having bog structure and preparation method therefor |
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| CN104591202A (en) * | 2013-11-04 | 2015-05-06 | 中国石油化工股份有限公司 | Hollow P type zeolite and preparation method thereof |
| CN104591202B (en) * | 2013-11-04 | 2016-03-30 | 中国石油化工股份有限公司 | A kind of hollow P type zeolite and preparation method thereof |
| CN103787356A (en) * | 2014-01-24 | 2014-05-14 | 东南大学 | Preparation method for hierarchical pore P-type molecular sieve |
| CN104528755A (en) * | 2014-12-26 | 2015-04-22 | 上海大学 | Method for preparing P1-type molecular sieve |
| CN106745058B (en) * | 2016-12-28 | 2019-09-10 | 河南大学 | A kind of microwave preparation of p-zeolite |
| CN106745058A (en) * | 2016-12-28 | 2017-05-31 | 河南大学 | A kind of microwave preparation of p-type molecular sieve |
| WO2018218736A1 (en) * | 2017-06-02 | 2018-12-06 | 中山大学 | Aluminosilicate zeolite molecular sieve having bog structure and preparation method therefor |
| CN107381524A (en) * | 2017-08-15 | 2017-11-24 | 中国神华能源股份有限公司 | The method and NaP molecular sieves of NaP molecular sieves are prepared using white clay as raw material |
| CN107381524B (en) * | 2017-08-15 | 2019-08-20 | 中国神华能源股份有限公司 | The method and NaP molecular sieve of NaP molecular sieve are prepared using white clay as raw material |
| CN108246239A (en) * | 2018-02-12 | 2018-07-06 | 东北石油大学 | The method of metal-doped KP types adsorbent of molecular sieve removing carbonyl sulfur |
| CN108246239B (en) * | 2018-02-12 | 2020-11-17 | 东北石油大学 | Method for removing carbonyl sulfide by metal-doped KP type molecular sieve adsorbent |
| CN112573536A (en) * | 2019-09-30 | 2021-03-30 | 中国石油化工股份有限公司 | Nano P-type zeolite, preparation method and application thereof |
| CN113522349A (en) * | 2021-07-28 | 2021-10-22 | 青岛科技大学 | Nitrogen-doped carbon-coated molecular sieve supported ruthenium catalyst, and preparation method and application thereof |
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