CN101863492A - Synthesis method of 4A-type zeolite - Google Patents
Synthesis method of 4A-type zeolite Download PDFInfo
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- CN101863492A CN101863492A CN 201010207907 CN201010207907A CN101863492A CN 101863492 A CN101863492 A CN 101863492A CN 201010207907 CN201010207907 CN 201010207907 CN 201010207907 A CN201010207907 A CN 201010207907A CN 101863492 A CN101863492 A CN 101863492A
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Abstract
The invention belongs to the technical field of an inorganic compound having the characteristic of molecular sieve, and relates to a synthesis method of 4A-type zeolite, in particular to a method for synthesizing the 4A-type zeolite by taking quartz sand as a silicon source. The method adopts natural ore the main component of which is silicon oxide to be as the silicon source, and comprises the synthesis steps of: activating silicon oxide in the silicon source by strong base solution under the conditions of 150-250 DEG C and 1-2MPa; preparing crystallized mixture containing SiO2, Al2O3, Na2O and H2O, and controlling the molar ratio among SiO2, Al2O3, Na2O and H2O to be 1.8- 2.2: 1: (3-4): (90-200); and carrying out hydrothermal crystallization on the crystallized mixture, and synthesizing the 4A-type zeolite. The content of the SiO2 in the quartz sand reaches more than 99.5%, and the impurity is less. By adopting the quartz sand as the silicon source, the method avoids impurity interference, omits the step of mineral impurity removal, and reduces the working procedures; and the price of the natural quartz sand is low, so that the cost is reduced.
Description
[technical field]
The invention belongs to the mineral compound technical field with property of the molecular sieve, relate to a kind of synthetic method of 4A type zeolite, particularly a kind of is the method for silicon source synthesis of 4a zeolite with quartz sand.
[background technology]
4A type zeolite is a kind of zeolitic material of synthetic, and it consists of Na
12Al
12Si
12O
4827H
2O belongs to isometric system, and the aperture is about 0.4nm.4A type zeolite all has important use in a plurality of fields: with 4A type zeolite is that the articles for washing of auxiliary agent has without phosphorus, no chemical pollution, noresidue, characteristics that soil removability is strong, has very extensively and important use in the washing industry; In the catalysis industry, 4A type zeolite is widely used in the petroleum cracking reaction; In the gas delivery industry, 4A type zeolite is used to prepare the sorbent material of high-purity gas.
The raw material sources of synthesis of 4a zeolite mainly contain two classes at present: the one, and chemical feedstocks mainly is water glass, sodium aluminate and sodium hydroxide; The 2nd, natural mineral raw is as kaolin, wilkinite, coal gangue or natural parastilbite etc.The chemical feedstocks method is produced the technical maturity of 4A type zeolite, and method is simple, but raw materials cost particularly silicon source cost is very high, deficiency in economic performance is unwell to large-scale industrial production.The synthetic zeolite molecular sieve raw materials cost that obtains of natural mineral method is cheap, but because natural mineral raw purity is limited, preparation method's complexity, the quality product that obtains simultaneously is also relatively poor.
[summary of the invention]
Purpose of the present invention is exactly in order to solve above-mentioned technical problem, proposed to adopt cheap, but SiO
2The higher quartz sand of content is as the method for silicon source synthesis of 4a zeolite.The main component of quartz sand is a silicon-dioxide, and content can reach more than 99.5%, and low price, with quartz sand be silicon source synthesis of 4a zeolite not only raw materials cost is cheap, and technology is simple, obtains the quality product height, helps large-scale industrial production.
Concrete technical scheme of the present invention is as follows:
The invention provides a kind of synthetic method of 4A type zeolite, it is that the natural crystal of silicon oxide is the silicon source that this method adopts main component, and synthesis step comprises: the silicon oxide in the silicon source is activated under 150 ℃～250 ℃ and 1～2MPa condition with strong base solution; Make and contain SiO
2, Al
2O
3, Na
2O and H
2The crystallization compound of O, and make SiO
2, Al
2O
3, Na
2O and H
2The mol ratio of O is 1.8～2.2: 1: (3～4): (90～200); The crystallization compound is carried out the hydrothermal crystallizing synthesis of 4a zeolite.
The synthesis step of this method is as follows:
The natural crystal, sodium hydroxide and the water that with main component are silicon oxide are that 1: 1.8～2.9: 2～8 ratio is packed in the sealed reaction device according to weight ratio, 150 ℃～250 ℃ reactions 2～8 hours down, make the alkali lye that contains active silica;
An amount of aluminium source dissolved in make aluminiferous solution in the water;
An amount of alkali lye that contains active silica is added in the aluminiferous solution, make SiO in the compound
2, Al
2O
3, Na
2O and H
2The mol ratio of O is 1.8～2.2: 1: (3～4): (90～200), and stirring makes the crystallization compound;
The crystallization compound is moved in the reactor in 80 ℃～120 ℃ crystallization 1～8 hour, filter then, wash, drying obtains 4A type zeolite.
This method further concrete steps is as follows:
The natural crystal, sodium hydroxide and the water that with main component are silicon oxide are that 1: 1.8～2.9: 2～8 ratio is packed in the autoclave according to weight ratio, startup is stirred and made rotating speed is 200～400 rev/mins, be warming up to 150 ℃～250 ℃, continued stirring reaction 2～8 hours, stop heating, stop after logical water coolant makes temperature in the kettle reduce to 40～50 ℃ stirring, make the alkali lye that contains active silica;
An amount of aluminium source dissolved in make aluminiferous solution in the water;
Under agitation condition, an amount of solution that contains active silica is added in the aluminiferous solution, make SiO in the compound
2, Al
2O
3, Na
2O and H
2The mol ratio of O is 1.8～2.2: 1: (3～4): (90～200), and continue stirring and made the crystallization compound in 20～40 minutes;
The crystallization compound is moved in the reactor, startup is stirred and made rotating speed is 100～300 rev/mins, and be warming up to 80 ℃～120 ℃ crystallization 1～8 hour, and stopped to stir after stopping to heat postcooling to 40 ℃～60 ℃, filter then, wash, drying obtains 4A type zeolite.
The another kind of synthesis step that this method adopts is as follows:
The natural crystal, sodium hydroxide and the water that with main component are silicon oxide are that 1: 1～2.9: 2～8 ratio is packed in the sealed reaction device according to weight ratio, 150 ℃～250 ℃ reactions 2～8 hours down, make the alkali lye that contains active silica;
An amount of aluminium source and sodium hydroxide dissolved in make aluminiferous basic solution in the water;
An amount of alkali lye that contains active silica is added in the aluminiferous basic solution, make SiO in the compound
2, Al
2O
3, Na
2O and H
2The mol ratio of O is 1.8～2.2: 1: (3～4): (90～200), and stirring makes the crystallization compound;
The crystallization compound is moved in the reactor in 80 ℃～120 ℃ crystallization 1～8 hour, filter then, wash, drying obtains 4A type zeolite.
This method further concrete steps is as follows:
The natural crystal, sodium hydroxide and the water that with main component are silicon oxide are that 1: 1～2.9: 2～8 ratio is packed in the autoclave according to weight ratio, startup is stirred and made rotating speed is 200～400 rev/mins, be warming up to 150 ℃～250 ℃, continued stirring reaction 2～8 hours, stop heating, stop after logical water coolant makes temperature in the kettle reduce to 40～50 ℃ stirring, make the alkali lye that contains active silica;
An amount of aluminium source and sodium hydroxide dissolved in make aluminiferous basic solution in the water;
Under agitation condition, an amount of alkali lye that contains active silica is added in the aluminiferous basic solution, make SiO in the compound
2, Al
2O
3, Na
2O and H
2The mol ratio of O is 1.8～2.2: 1: (3～4): (90～200), and continue stirring and made the crystallization compound in 20～40 minutes;
The crystallization compound is moved in the reactor, startup is stirred and made rotating speed is 100～300 rev/mins, and be warming up to 80 ℃～120 ℃ crystallization 1～8 hour, and stopped to stir after stopping to heat postcooling to 40 ℃～60 ℃, filter then, wash, drying obtains 4A type zeolite.
Described main component is that the natural crystal of silicon oxide is a quartz sand.
Described aluminium source is a kind of compound or the multiple mixture in sodium aluminate, Tai-Ace S 150, aluminum nitrate, aluminum chloride, aluminum phosphate and the aluminum isopropylate.
The particle diameter of described quartz sand is less than 100 orders.
Beneficial technical effects of the present invention is:
The content of silicon-dioxide has reached more than 99.5% in the quartz sand, and impurity is few, and it is the silicon source that the present invention adopts quartz sand, has avoided the impurity interference, has saved mineral removal of impurity step, has reduced operation, and the natural siliceous sand low price, has reduced cost.
The overwhelming majority is a silicon-dioxide in the quartz sand, so raw material availability height of the present invention.
The 4A type zeolite that synthesizes has the degree of crystallinity height, whiteness height, the characteristics of size distribution homogeneous.
[embodiment]
The present invention relates to a kind of is the method for silicon source synthesis of 4a zeolite with quartz sand.
The invention will be further elaborated and explanation below by specific embodiment:
Embodiment 1
Adopting Heyuan area quartz sand is the silicon source, SiO
2Content is 99.8%, and particle diameter is 100～200 orders.With 360g quartz sand, 360g sodium hydroxide, 720mL water once add in the autoclave, and startup is stirred and made rotating speed is 200 rev/mins, are warming up to 150 degree, continue to stir 2 hours.Stop heating, logical water coolant stops to stir after making temperature in the kettle reduce to 40 degree, takes out reactant, obtains the active silica alkali lye of clear.447g sodium metaaluminate and 294.5g sodium hydroxide are dissolved in 3698 ml waters.Under agitation condition active silica alkali lye is added in the sodium aluminate solution then, continue to stir 20 minutes, obtain the crystallization compound, this moment, the molar ratio of material of compound was: SiO
2: Al
2O
3: Na
2O: H
2O=2.2: 1: 3: 90.The crystallization compound is moved in the 10L reactor, start and stir (100 rev/mins), be warming up to 80 degree again, crystallization 1 hour stops heating, and logical water coolant makes temperature of reaction kettle reduce to 40 degree, drive still after stopping to stir, material in the still is carried out suction filtration, washing, drying obtains product under 120 degree conditions then.This product detects through " X-ray diffraction analysis ", and the major ingredient of sample is the 4A zeolite, and degree of crystallinity is 96%, and whiteness is 97%, and particle diameter is 2～3 μ m, Ca
2+Exchange capacity is 322mg/g.
Embodiment 2
The quartz sand raw material is with embodiment 1.
With 360g quartz sand, 416g sodium hydroxide, 1300mL water once add in the autoclave, and startup is stirred and made rotating speed is 300 rev/mins, are warming up to 200 degree, continue to stir 4 hours.Stop heating, logical water coolant stops to stir after making temperature in the kettle reduce to 45 degree, takes out reactant, obtains the active silica alkali lye of clear.492g sodium metaaluminate and 424g sodium hydroxide are dissolved in 4100 ml waters.Under agitation condition active silica alkali lye is added in the sodium aluminate solution then, continue to stir 30 minutes, obtain the crystallization compound, this moment, the molar ratio of material of compound was: SiO
2: Al
2O
3: Na
2O: H
2O=2: 1: 3.5: 100.The crystallization compound is moved in the 20L reactor, start and stir (200 rev/mins), be warming up to 100 degree again, crystallization 3 hours stops heating, and logical water coolant makes temperature of reaction kettle reduce to 50 degree, drive still after stopping to stir, material in the still is carried out suction filtration, washing, drying obtains product under 120 degree conditions then.This product detects through " X-ray diffraction analysis ", and the major ingredient of sample is the 4A zeolite, and degree of crystallinity is 94%, and whiteness is 97%, and particle diameter is 1.5～2.5 μ m, Ca
2+Exchange capacity is 317mg/g.
Embodiment 3
The quartz sand raw material is with embodiment 1.
With 360g quartz sand, 1044g sodium hydroxide, 1300mL water once add in the autoclave, and startup is stirred and made rotating speed is 400 rev/mins, are warming up to 250 degree, continue to stir 8 hours.Stop heating, logical water coolant stops to stir after making temperature in the kettle reduce to 50 degree, takes out reactant, obtains the active silica alkali lye of clear.547g sodium metaaluminate and 22g sodium hydroxide are dissolved in 10700 ml waters.Under agitation condition active silica alkali lye is added in the sodium aluminate solution then, continue to stir 40 minutes, obtain the crystallization compound, this moment, the molar ratio of material of compound was: SiO
2: Al
2O
3: Na
2O: H
2O=1.8: 1: 4: 200.The crystallization compound is moved in the 20L reactor, start and stir (300 rev/mins), be warming up to 120 degree again, crystallization 8 hours stops heating, and logical water coolant makes temperature of reaction kettle reduce to 50 degree, drive still after stopping to stir, material in the still is carried out suction filtration, washing, drying obtains product under 120 degree conditions then.This product detects through " X-ray diffraction analysis ", and the major ingredient of sample is the 4A zeolite, and degree of crystallinity is 92%, and whiteness is 97%, and particle diameter is 1.5～2.5 μ m, Ca
2+Exchange capacity is 312mg/g.
Embodiment 4
The quartz sand raw material is with embodiment 1.
With 360g quartz sand, 648g sodium hydroxide, 720mL water once add in the autoclave, and startup is stirred and made rotating speed is 300 rev/mins, are warming up to 200 degree, continue to stir 5 hours.Stop heating, logical water coolant stops to stir after making temperature in the kettle reduce to 50 degree, takes out reactant, obtains the active silica alkali lye of clear.The 447g sodium metaaluminate is dissolved in 3695 ml waters.Under agitation condition active silica alkali lye is added in the sodium aluminate solution then, continue to stir 30 minutes, obtain the crystallization compound, this moment, the molar ratio of material of compound was: SiO
2: Al
2O
3: Na
2O: H
2O=2.2: 1: 3: 90.The crystallization compound is moved in the 10L reactor, start and stir (200 rev/mins), be warming up to 100 degree again, crystallization 3 hours stops heating, and logical water coolant is reduced to below 50 degree temperature of reaction kettle, drive still after stopping to stir, material in the still is carried out suction filtration, washing, drying obtains product under 120 degree conditions then.This product detects through " X-ray diffraction analysis ", and the major ingredient of sample is the 4A zeolite, and degree of crystallinity is 93%, and whiteness is 97%, and particle diameter is 1.5～3.0 μ m, Ca
2+Exchange capacity is 316mg/g.
Embodiment 5
The quartz sand raw material is with embodiment 1.
With 360g quartz sand, 1044g sodium hydroxide, 2880mL water once add in the autoclave, and startup is stirred and made rotating speed is 300 rev/mins, are warming up to 180 degree, continue to stir 4 hours.Stop heating, logical water coolant stops to stir after making temperature in the kettle reduce to 50 degree, takes out reactant, obtains the active silica alkali lye of clear.The 547g sodium metaaluminate is dissolved in 9127 ml waters.Under agitation condition active silica alkali lye is added in the sodium aluminate solution then, continue to stir 30 minutes, obtain the crystallization compound, this moment, the molar ratio of material of compound was: SiO
2: Al
2O
3: Na
2O: H
2O=1.8: 1: 4: 200.The crystallization compound is moved in the 10L reactor, start and stir (200 rev/mins), be warming up to 100 degree again, crystallization 3 hours stops heating, and logical water coolant is reduced to below 50 degree temperature of reaction kettle, drive still after stopping to stir, material in the still is carried out suction filtration, washing, drying obtains product under 100 degree conditions then.This product detects through " X-ray diffraction analysis ", and the major ingredient of sample is the 4A zeolite, and degree of crystallinity is 98%, and whiteness is 97%, and particle diameter is 1.5～2.5 μ m, Ca
2+Exchange capacity is 325mg/g.
Need to prove that the above embodiments are the explanations to claims of the present invention; and it is unrestricted; those skilled in the art is according to principle of the present invention and design; again in conjunction with embodiments of the invention; can be easy to the improvement of arriving other of association and the technical scheme of distortion; no matter how it improves and is out of shape, if with principle of the present invention and conceive identical, all should be within protection scope of the present invention.
Claims (8)
1. it is that the natural crystal of silicon oxide is the silicon source that the synthetic method of a 4A type zeolite, this method adopt main component, and synthesis step comprises: the silicon oxide in the silicon source is activated under 150 ℃～250 ℃ and 1～2MPa condition with strong base solution; Make and contain SiO
2, Al
2O
3, Na
2O and H
2The crystallization compound of O, and make SiO
2, Al
2O
3, Na
2O and H
2The mol ratio of O is 1.8～2.2: 1: (3～4): (90～200); The crystallization compound is carried out the hydrothermal crystallizing synthesis of 4a zeolite.
2. the synthetic method of 4A type zeolite according to claim 1 is characterized in that, the synthesis step of this method is as follows:
The natural crystal, sodium hydroxide and the water that with main component are silicon oxide are that 1: 1.8～2.9: 2～8 ratio is packed in the sealed reaction device according to weight ratio, 150 ℃～250 ℃ reactions 2～8 hours down, make the alkali lye that contains active silica;
An amount of aluminium source dissolved in make aluminiferous solution in the water;
An amount of alkali lye that contains active silica is added in the aluminiferous solution, make SiO in the compound
2, Al
2O
3, Na
2O and H
2The mol ratio of O is 1.8～2.2: 1: (3～4): (90～200), and stirring makes the crystallization compound;
The crystallization compound is moved in the reactor in 80 ℃～120 ℃ crystallization 1～8 hour, filter then, wash, drying obtains 4A type zeolite.
3. the synthetic method of 4A type zeolite according to claim 2 is characterized in that, this method further concrete steps is as follows:
The natural crystal, sodium hydroxide and the water that with main component are silicon oxide are that 1: 1.8～2.9: 2～8 ratio is packed in the autoclave according to weight ratio, startup is stirred and made rotating speed is 200～400 rev/mins, be warming up to 150 ℃～250 ℃, continued stirring reaction 2～8 hours, stop heating, stop after logical water coolant makes temperature in the kettle reduce to 40～50 ℃ stirring, make the alkali lye that contains active silica;
An amount of aluminium source dissolved in make aluminiferous solution in the water;
Under agitation condition, an amount of solution that contains active silica is added in the aluminiferous solution, make SiO in the compound
2, Al
2O
3, Na
2O and H
2The mol ratio of O is 1.8～2.2: 1: (3～4): (90～200), and continue stirring and made the crystallization compound in 20～40 minutes;
The crystallization compound is moved in the reactor, startup is stirred and made rotating speed is 100～300 rev/mins, and be warming up to 80 ℃～120 ℃ crystallization 1～8 hour, and stopped to stir after stopping to heat postcooling to 40 ℃～60 ℃, filter then, wash, drying obtains 4A type zeolite.
4. the synthetic method of 4A type zeolite according to claim 1 is characterized in that, the synthesis step that this method adopts is as follows:
The natural crystal, sodium hydroxide and the water that with main component are silicon oxide are that 1: 1～2.9: 2～8 ratio is packed in the sealed reaction device according to weight ratio, 150 ℃～250 ℃ reactions 2～8 hours down, make the alkali lye that contains active silica;
An amount of aluminium source and sodium hydroxide dissolved in make aluminiferous basic solution in the water;
An amount of alkali lye that contains active silica is added in the aluminiferous basic solution, make SiO in the compound
2, Al
2O
3, Na
2O and H
2The mol ratio of O is 1.8～2.2: 1: (3～4): (90～200), and stirring makes the crystallization compound;
The crystallization compound is moved in the reactor in 80 ℃～120 ℃ crystallization 1～8 hour, filter then, wash, drying obtains 4A type zeolite.
5. the synthetic method of 4A type zeolite according to claim 4 is characterized in that, this method further concrete steps is as follows:
The natural crystal, sodium hydroxide and the water that with main component are silicon oxide are that 1: 1～2.9: 2～8 ratio is packed in the autoclave according to weight ratio, startup is stirred and made rotating speed is 200～400 rev/mins, be warming up to 150 ℃～250 ℃, continued stirring reaction 2～8 hours, stop heating, stop after logical water coolant makes temperature in the kettle reduce to 40～50 ℃ stirring, make the alkali lye that contains active silica;
An amount of aluminium source and sodium hydroxide dissolved in make aluminiferous basic solution in the water;
Under agitation condition, an amount of alkali lye that contains active silica is added in the aluminiferous basic solution, make SiO in the compound
2, Al
2O
3, Na
2O and H
2The mol ratio of O is 1.8～2.2: 1: (3～4): (90～200), and continue stirring and made the crystallization compound in 20～40 minutes;
The crystallization compound is moved in the reactor, startup is stirred and made rotating speed is 100～300 rev/mins, and be warming up to 80 ℃～120 ℃ crystallization 1～8 hour, and stopped to stir after stopping to heat postcooling to 40 ℃～60 ℃, filter then, wash, drying obtains 4A type zeolite.
6. according to the synthetic method of the arbitrary described 4A type zeolite of claim 1-5, it is characterized in that described main component is that the natural crystal of silicon oxide is a quartz sand.
7. according to the synthetic method of the arbitrary described 4A type zeolite of claim 1-5, it is characterized in that described aluminium source is a kind of compound or the multiple mixture in sodium aluminate, Tai-Ace S 150, aluminum nitrate, aluminum chloride, aluminum phosphate and the aluminum isopropylate.
8. the synthetic method of 4A type zeolite according to claim 6 is characterized in that the particle diameter of described quartz sand is less than 100 orders.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102583429A (en) * | 2012-02-17 | 2012-07-18 | 中国地质大学（北京） | Method for synthesizing 4A-type molecular sieve by utilizing aluminum-silicon tailings obtained in process of carrying out potassium extraction on potassium feldspar |
| CN104229816A (en) * | 2014-09-11 | 2014-12-24 | 上海化工研究院 | Organic/inorganic complex zeolite material and preparation method thereof |
| CN106830000A (en) * | 2017-01-20 | 2017-06-13 | 宁夏大学 | A kind of synthetic method of the molecular sieves of bundle shape HZSM 48 |
| CN109137074A (en) * | 2018-10-23 | 2019-01-04 | 梁维嘉 | The artificial culture growing method of quartzy embryo |
| CN111099611A (en) * | 2020-01-03 | 2020-05-05 | 厦门欣意盛新材料科技有限公司 | Method for synthesizing pure silicon zeolite by recycling mother liquor repeatedly |
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| US5000933A (en) * | 1989-01-31 | 1991-03-19 | Henkel Kommanditgesellschaft Auf Aktien | Process for hydrothermal production of sodium silicate solutions |
| CN1837042A (en) * | 2006-04-11 | 2006-09-27 | 云南盐化股份有限公司 | Process for industrial production of laminated sodium disilicate crystal with low cost |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102583429A (en) * | 2012-02-17 | 2012-07-18 | 中国地质大学（北京） | Method for synthesizing 4A-type molecular sieve by utilizing aluminum-silicon tailings obtained in process of carrying out potassium extraction on potassium feldspar |
| CN104229816A (en) * | 2014-09-11 | 2014-12-24 | 上海化工研究院 | Organic/inorganic complex zeolite material and preparation method thereof |
| CN106830000A (en) * | 2017-01-20 | 2017-06-13 | 宁夏大学 | A kind of synthetic method of the molecular sieves of bundle shape HZSM 48 |
| CN109137074A (en) * | 2018-10-23 | 2019-01-04 | 梁维嘉 | The artificial culture growing method of quartzy embryo |
| CN111099611A (en) * | 2020-01-03 | 2020-05-05 | 厦门欣意盛新材料科技有限公司 | Method for synthesizing pure silicon zeolite by recycling mother liquor repeatedly |
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