CN101618880A - Method for synthesizing pure 4A zeolite, P-shaped zeolite and sodalite with concavo-convex attapulgite clay - Google Patents
Method for synthesizing pure 4A zeolite, P-shaped zeolite and sodalite with concavo-convex attapulgite clay Download PDFInfo
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- CN101618880A CN101618880A CN200910182050A CN200910182050A CN101618880A CN 101618880 A CN101618880 A CN 101618880A CN 200910182050 A CN200910182050 A CN 200910182050A CN 200910182050 A CN200910182050 A CN 200910182050A CN 101618880 A CN101618880 A CN 101618880A
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Abstract
The invention discloses a method for synthesizing pure 4A zeolite, P-shaped zeolite and sodalite with concavo-convex attapulgite clay. The method is characterized by comprising the following steps: firstly, the concavo-convex attapulgite clay is calcined in high temperature; then, the calcined concavo-convex attapulgite clay is soaked by soda liquor to obtain leach liquor containing Na2SiO3; finally, an aluminum source is added into the soda leach liquor to carry out hydrothermal crystallization synthesis, and then, the pure 4A zeolite, the P-shaped zeolite and the sodalite are respectively obtained by filtration, rinsing and drying. In the method, the concavo-convex attapulgite clay is used as raw material, and the genuine 4A zeolite, the P-shaped zeolite and the sodalite are respectively obtained by calcination and soda-leach pretreatment through adjusting synthesis conditions, therefore the invention has the advantages of simple synthesis method, easily obtained raw material and low production cost.
Description
Technical field
The present invention relates to a kind of is the method for synthetic pure 4A zeolite, P type zeolite and sodalite of raw material with the attapulgite clay, specifically a kind of is the silicon source with the calcined attapulgite clay, by regulating the synthesis condition method of synthetic pure 4A zeolite, P type zeolite and sodalite respectively.
Background technology
Zeolite be have regular duct, than the aluminosilicate crystal of bigger serface, high hydrothermal stability, be widely used in fields such as catalysis, absorption, separation.Wherein 4A zeolite and P type zeolite have stronger ion-exchange capacity, are the good substitutes of washing auxiliary detergent tripoly phosphate sodium STPP, also can be used as sorbent material, siccative etc.; Sodalite is a kind ofly to have
The porous silicoaluminate zeolite in aperture can be used as sorbent material, photochromic material and hydrogen storage material, has big prospects for commercial application.Above-mentioned zeolite can be synthetic by the industrial chemicals that contains aluminium or silicon and sodium hydroxide hydro-thermal, the purity height, and quality is better, however production cost is higher, and raw material sources are restricted, and have restricted the Application Areas of synthetic zeolite.Therefore, in order to reduce production costs, adopt the inorganic mineral of silicon-aluminum containing, as kaolin (ZL98117045.5, CN101033070A), flyash (ZL02138756.7, ZL02112272.5), coal gangue (ZL200410064592.X), bauxite (nonmetalliferous ore, 2008,24～26), wilkinite (CN101428815A) waits to synthesize above-mentioned zeolite, to replace traditional industrial chemicals, formed certain industrial scale at present.
Attapulgite clay (hereinafter to be referred as recessed soil) be a kind of layer of chain-like structure contain Shuifu County's zeopan clay mineral, the theoretical chemistry composition is: SiO
256.96%, (Fe) O 23.83%, H for Mg, Al
2O 19.21%; Contain more SiO in the recessed soil
2Composition, therefore recessed soil can be used as the silicon source of zeolite synthesis.Be that raw material soaks processing by hydro-thermal alkali and can synthesize euthalite, mordenite, A type zeolite (CN101066766A) and X type zeolite (CN101337681A) with it at present.
Summary of the invention
The objective of the invention is: the method that synthetic pure 4A zeolite, P type zeolite and sodalite of a kind of attapulgite clay is provided, with inexpensive attapulgite clay is raw material, regulate synthesis condition synthetic respectively pure 4A zeolite, P type zeolite and sodalite, expand the using value of recessed soil.
Technical solution of the present invention is that this synthetic method may further comprise the steps: at first, and the high-temperature calcination attapulgite clay; Then, dipping by lye incinerating attapulgite clay must contain Na
2SiO
3Leach liquor; At last, adding the aluminium source in the alkaline leach liquor, to carry out hydrothermal crystallizing synthetic, after filtration, washing and drying obtain pure 4A zeolite, P type zeolite and sodalite respectively.
The concrete steps of synthetic method of the present invention are as follows:
1) 600～800 ℃ of roasting 1～3h of attapulgite clay;
2) the incinerating attapulgite clay is pressed the solid-liquid mass volume ratio and added dipping by lye at 1: 4, filter, must contain Na
2SiO
3Leach liquor; Wherein, alkali lye is concentration 5mol/L or 8mol/LNaOH solution, and treatment temp is 80～100 ℃, and the treatment time is 1～2h;
3) leach in the alkaline leach liquor obtain at 5mol/LNaOH solution and added aluminium source solution in 1: 1 by volume, stirring at room ageing 0.5h, 80～90 ℃ are carried out hydrothermal crystallizing 5h, and after filtration, washing and dry pure 4A zeolite, wherein, aluminium source solution is Al
2(SO
4)
3Or NaAlO
2Solution, Al
3+The ion volumetric molar concentration is 1～1.88mol/L; Or leach in the alkaline leach liquor obtain at 5mol/LNaOH solution and to add aluminium source solution in 1: 4 by volume, stir, with the H of 1mol/L
2SO
4Or HCl solution to regulate pH value be 11, stirring at room ageing 8～12h, 110～150 ℃ of hydrothermal crystallizing 8～48h, after filtration, washing and dry must P type zeolite, wherein, aluminium source solution is Al
2(SO
4)
3Or NaAlO
2Solution, Al
3+The ion volumetric molar concentration is 1～2.5mol/L; Or leach in the alkaline leach liquor obtain at 8mol/LNaOH solution and to add aluminium source solution in 1: 4 by volume, stirring at room ageing 8～12h, 180 ℃ of hydrothermal crystallizing 8～24h, after filtration, washing and dry sodalite, wherein, aluminium source solution is Al
2(SO
4)
3Or NaAlO
2Solution, Al
3+The ion volumetric molar concentration is 1～3mol/L.
Synthetic method of the present invention is raw material with the attapulgite clay, soaks pre-treatment through calcining, alkali, obtains pure 4A zeolite, P type zeolite and sodalite respectively by regulating synthesis condition, and synthetic method is simple, and raw material is easy to get, and production cost is low.
Description of drawings
Fig. 1 is the SEM photo of synthetic 4A zeolite of the present invention
Fig. 2 is the SEM photo of synthetic P type zeolite of the present invention
Fig. 3 is the SEM photo of synthetic sodalite of the present invention
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail; Should be understood that these embodiment are technical solution in order to demonstrate the invention, but not limit the scope of the invention by any way.
Embodiment 1
With the attapulgite clay is the pure 4A zeolite of feedstock production: at 800 ℃ of following calcined attapulgite clay 1h; 5g incinerating attapulgite clay is placed the NaOH solution of the 5mol/L of 20ml, and 100 ℃ are stirred 1h, filter, and obtain containing Na
2SiO
3Leach liquor; With 2.5gNaAlO
2Join 19.23g H
2Stir among the O, aluminium source solution is poured above-mentioned leach liquor into, stirs 0.5h, 80 ℃ of hydrothermal crystallizing 5h of mixed solution, after filtration, washing, dry product; The sample of product characterizes through XRD and SEM, is cubical pure 4A zeolite.
Embodiment 2
With the attapulgite clay is the pure 4A zeolite of feedstock production: at 700 ℃ of following calcined attapulgite clay 2h; 5g incinerating attapulgite clay is placed the NaOH solution of the 5mol/L of 20ml, and 90 ℃ are stirred 1.5h, filter, and obtain containing Na
2SiO
3Leach liquor; With 3.6gNaAlO
2Join 19.23g H
2Stir among the O, aluminium source solution is poured above-mentioned leach liquor into, stirs 0.5h, 85 ℃ of hydrothermal crystallizing 5h of mixed solution, after filtration, washing, dry product; The sample of product characterizes through XRD and SEM, is cubical pure 4A zeolite.
Embodiment 3
With the attapulgite clay is the pure 4A zeolite of feedstock production: at 600 ℃ of following calcined attapulgite clay 3h; 5g incinerating attapulgite clay is placed the NaOH solution of the 5mol/L of 20ml, and 85 ℃ are stirred 2h, filter, and obtain containing Na
2SiO
3Leach liquor; With 5.4gNaAlO
2Join 19.23g H
2Stir among the O, aluminium source solution is poured above-mentioned leach liquor into, stirs 0.5h, 90 ℃ of hydrothermal crystallizing 5h of mixed solution, after filtration, washing, dry product; The sample of product characterizes through XRD and SEM, is cubical pure 4A zeolite.
Embodiment 4
With the attapulgite clay is the pure 4A zeolite of feedstock production: the roasting of attapulgite clay and alkaline purification obtain containing Na with example 1
2SiO
3Leach liquor; With 6.66g Al
2(SO
4)
318H
2O joins 16g H
2Stir among the O, aluminium source solution is poured above-mentioned leach liquor into, stirs 0.5h, 80 ℃ of hydrothermal crystallizing 5h of mixed solution, after filtration, washing, dry product; The sample of product characterizes through XRD and SEM, is cubical pure 4A zeolite.
Embodiment 5
With the attapulgite clay is the pure 4A zeolite of feedstock production: the roasting of attapulgite clay and alkaline purification obtain containing Na with example 1
2SiO
3Leach liquor; With 10g Al
2(SO
4)
318H
2O joins 14.37g H
2Stir among the O, aluminium source solution is poured above-mentioned leach liquor into, stirs 0.5h, 90 ℃ of hydrothermal crystallizing 5h of mixed solution, after filtration, washing, dry product; The sample of product characterizes through XRD and SEM, is cubical pure 4A zeolite.
Embodiment 6
With the attapulgite clay is the pure P type of feedstock production zeolite: calcine recessed native 1h down at 800 ℃; 5g incinerating attapulgite clay is placed the NaOH solution of 20ml 5mol/L, and 100 ℃ are stirred 1h, filter, and obtain containing Na
2SiO
3Leach liquor; With 1.658gAl
2(SO
4)
318H
2O joins 5g H
2Stir among the O, aluminium source solution is poured above-mentioned leach liquor into, stirs 0.5h, uses 1mol/LH
2SO
4Solution is regulated pH=11, ageing 8h, and 110 ℃ of hydrothermal crystallizing 48h of mixed solution, after filtration, washing, dry product; The sample of product characterizes through XRD and SEM, is pure P type zeolite.
Embodiment 7
With the attapulgite clay is the pure P type of feedstock production zeolite: calcine recessed native 2h down at 700 ℃; 5g incinerating attapulgite clay is placed the NaOH solution of 20ml 5mol/L, and 90 ℃ are stirred 1.5h, filter, and obtain containing Na
2SiO
3Leach liquor; With 2.82gAl
2(SO
4)
318H
2O joins 5g H
2Stir among the O, aluminium source solution is poured above-mentioned leach liquor into, stirs 0.5h, uses 1mol/LH
2SO
4Solution is regulated its pH=11, ageing 10h, and 130 ℃ of following hydrothermal crystallizing 24h, after filtration, washing, dry product; The sample of product characterizes through XRD and SEM, is pure P type zeolite.
Embodiment 8
With the attapulgite clay is the pure P type of feedstock production zeolite: calcine recessed native 3h down at 600 ℃; 5g incinerating attapulgite clay is placed the NaOH solution of 20ml 5mol/L, and 80 ℃ are stirred 2h, filter, and obtain containing Na
2SiO
3Leach liquor; With 4.14gAl
2(SO
4)
318H
2O joins the H of 5g
2Stir among the O, aluminium source solution is poured above-mentioned leach liquor into, stirs 0.5h, regulates its pH=11 with 1mol/LHCl solution, ageing 12h, 150 ℃ of hydrothermal crystallizing 8h of mixed solution, after filtration, washing, dry must product; The sample of product characterizes through XRD and SEM, is pure P type zeolite.
Embodiment 9
With the attapulgite clay is the pure P type of feedstock production zeolite: the roasting of attapulgite clay and alkaline purification obtain containing Na with example 6
2SiO
3Leach liquor; With 0.62gNaAlO
2Join the H of 5g
2Stir among the O, aluminium source solution is poured above-mentioned leach liquor into, stirs 0.5h, regulates its pH=11 with 1mol/LHCl solution, ageing 12h, 150 ℃ of hydrothermal crystallizing 24h of mixed solution, after filtration, washing, dry must product; The sample of product characterizes through XRD and SEM, is pure P type zeolite.
Embodiment 10
With the attapulgite clay is the pure P type of feedstock production zeolite: the roasting of attapulgite clay and alkaline purification obtain containing Na with example 6
2SiO
3Leach liquor; With 1.55gNaAlO
2Join the H of 5g
2Stir among the O, aluminium source solution is poured above-mentioned leach liquor into, stirs 0.5h, regulates its pH=11 with 1mol/LHCl solution, ageing 12h, 110 ℃ of hydrothermal crystallizing 36h of mixed solution, after filtration, washing, dry must product; The sample of product characterizes through XRD and SEM, is pure P type zeolite.
Embodiment 11
With the attapulgite clay is the feedstock production sodalite: calcine recessed native 1h down at 800 ℃; 6.25g incinerating attapulgite clay is placed the NaOH solution of 25ml 8mol/L, and 100 ℃ are stirred 1h down, filter, and obtain containing Na
2SiO
3Leach liquor; With 1.8gAl
2(SO
4)
318H
2O joins the H of 5g
2Stir among the O, aluminium source solution is poured above-mentioned leach liquor into, ageing 8h, and 180 ℃ of hydrothermal crystallizing 8h of mixed solution, after filtration, washing, dry product; The sample of product characterizes through XRD and SEM, is sodalite.
Embodiment 12
With the attapulgite clay is the feedstock production sodalite: calcine recessed native 2h down at 700 ℃; 6.25g incinerating attapulgite clay is placed the NaOH solution of 25ml 8mol/L, and 90 ℃ are stirred 1.5h down, filter, and obtain containing Na
2SiO
3Leach liquor; With 3.6gAl
2(SO
4)
318H
2O joins the H of 5g
2Stir among the O, aluminium source solution is poured above-mentioned leach liquor into, ageing 10h, and 180 ℃ of hydrothermal crystallizing 16h of mixed solution, after filtration, washing, dry product; The sample of product characterizes through XRD and SEM, is sodalite.
Embodiment 13
With the attapulgite clay is the feedstock production sodalite: calcine recessed native 3h down at 600 ℃; 6.25g incinerating attapulgite clay is placed the NaOH solution of 25ml 8mol/L, and 80 ℃ are stirred 2h down, filter, and obtain containing Na
2SiO
3Leach liquor; With 5.4gAl
2(SO
4)
318H
2O joins the H of 5g
2Stir among the O, aluminium source solution is poured above-mentioned leach liquor into, ageing 24h, and 180 ℃ of hydrothermal crystallizing 24h of mixed solution, after filtration, washing, dry product; The sample of product characterizes through XRD and SEM, is sodalite.
Embodiment 14
With the attapulgite clay is the feedstock production sodalite: the roasting of attapulgite clay and alkaline purification obtain containing Na with example 11
2SiO
3Leach liquor; With 0.67gNaAlO
2Join the H of 5g
2Stir among the O, aluminium source solution is poured above-mentioned leach liquor into, ageing 24h, and 180 ℃ of hydrothermal crystallizing 24h of mixed solution, after filtration, washing, dry product; The sample of product characterizes through XRD and SEM, is sodalite.
Embodiment 15
With the attapulgite clay is the feedstock production sodalite: the roasting of attapulgite clay and alkaline purification obtain containing Na with example 11
2SiO
3Leach liquor; With 2.02gNaAlO
2Join the H of 5g
2Stir among the O, aluminium source solution is poured above-mentioned leach liquor into, ageing 10h, and 180 ℃ of hydrothermal crystallizing 24h of mixed solution, after filtration, washing, dry product; The sample of product characterizes through XRD and SEM, is sodalite.
Claims (2)
1, the method for synthetic pure 4A zeolite, P type zeolite and sodalite of attapulgite clay is characterized in that this synthetic method may further comprise the steps: at first, and the high-temperature calcination attapulgite clay; Then, dipping by lye incinerating attapulgite clay must contain Na
2SiO
3Leach liquor; At last, adding the aluminium source in the alkaline leach liquor, to carry out hydrothermal crystallizing synthetic, after filtration, washing and drying obtain pure 4A zeolite, P type zeolite, sodalite respectively.
2, the method for synthetic pure 4A zeolite, P type zeolite and sodalite of attapulgite clay according to claim 1 is characterized in that the concrete steps of synthetic method are as follows:
1) 600～800 ℃ of roasting 1～3h of attapulgite clay;
2) the incinerating attapulgite clay is pressed the solid-liquid mass volume ratio and added dipping by lye at 1: 4, filter, must contain Na
2SiO
3Leach liquor; Wherein, alkali lye is concentration 5mol/L or 8mol/LNaOH solution, and treatment temp is 80～100 ℃, and the treatment time is 1～2h;
3) leach in the alkaline leach liquor obtain at 5mol/LNaOH solution and added aluminium source solution in 1: 1 by volume, stirring at room ageing 0.5h, 80～90 ℃ are carried out hydrothermal crystallizing 5h, and after filtration, washing and dry pure 4A zeolite, wherein, aluminium source solution is Al
2(SO
4)
3Or NaAlO
2Solution, Al
3+The ion volumetric molar concentration is 1～1.88mol/L; Or leach in the alkaline leach liquor obtain at 5mol/LNaOH solution and to add aluminium source solution in 1: 4 by volume, stir, with the H of 1mol/L
2SO
4Or HCl solution to regulate pH value be 11, stirring at room ageing 8～12h, 110～150 ℃ of hydrothermal crystallizing 8～48h, after filtration, washing and dry must P type zeolite, wherein, aluminium source solution is Al
2(SO
4)
3Or NaAlO
2Solution, Al
3+The ion volumetric molar concentration is 1～2.5mol/L; Leach in the alkaline leach liquor obtain at 8mol/LNaOH solution and to add aluminium source solution in 1: 4 by volume, stirring at room ageing 8～12h, 180 ℃ of hydrothermal crystallizing 8～24h, after filtration, washing and dry sodalite, wherein, aluminium source solution is Al
2(SO
4)
3Or NaAlO
2Solution, Al
3+The ion volumetric molar concentration is 1～3mol/L.
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| CN102659133A (en) * | 2012-04-20 | 2012-09-12 | 华东师范大学 | Preparation method for P type zeolite molecular sieve with core-shell structure |
| CN103626194A (en) * | 2013-12-03 | 2014-03-12 | 西南科技大学 | Sodalite synthesis method by adopting bentonite through one-step alkali dissolution |
| CN104528748A (en) * | 2015-01-16 | 2015-04-22 | 中国地质大学（武汉） | Method for synthesizing SOD type sodalite in low-temperature controllable manner |
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| CN105858674A (en) * | 2016-03-28 | 2016-08-17 | 大唐国际发电股份有限公司高铝煤炭资源开发利用研发中心 | Method for preparing sodalite by utilizing high-alumina fly ash |
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| CN103626194A (en) * | 2013-12-03 | 2014-03-12 | 西南科技大学 | Sodalite synthesis method by adopting bentonite through one-step alkali dissolution |
| CN104528748A (en) * | 2015-01-16 | 2015-04-22 | 中国地质大学（武汉） | Method for synthesizing SOD type sodalite in low-temperature controllable manner |
| CN104556117A (en) * | 2015-01-28 | 2015-04-29 | 西安科技大学 | Method for preparing 4A molecular sieve by adopting coal slime |
| CN104556117B (en) * | 2015-01-28 | 2016-08-17 | 西安科技大学 | A kind of method using coal slime to prepare 4A type molecular sieve |
| CN105858674B (en) * | 2016-03-28 | 2018-03-02 | 大唐国际发电股份有限公司高铝煤炭资源开发利用研发中心 | A kind of method that sodalite is prepared using aluminous fly-ash |
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| CN106745054A (en) * | 2016-12-16 | 2017-05-31 | 西京学院 | A kind of preparation method of the molecular sieves of ZSM 5 |
| CN107055565A (en) * | 2017-05-31 | 2017-08-18 | 合肥工业大学 | A kind of method that zeolite molecular sieve is prepared with opal attapulgite clay |
| CN107055565B (en) * | 2017-05-31 | 2019-08-02 | 合肥工业大学 | A method of zeolite molecular sieve is prepared with opal attapulgite clay |
| CN108516565B (en) * | 2018-05-17 | 2021-06-25 | 中南大学 | Method for preparing P-type zeolite molecular sieve by using aluminum calcium powder reaction slag |
| CN108516565A (en) * | 2018-05-17 | 2018-09-11 | 中南大学 | A method of preparing P type zeolite molecular sieve using aluminium calcium powder reaction slag |
| CN108408739A (en) * | 2018-06-04 | 2018-08-17 | 陕西师范大学 | A method of using gangue be raw material two-step method hydrothermal synthesis sodalite |
| CN109292792A (en) * | 2018-09-07 | 2019-02-01 | 昆明理工大学 | A kind of method that twin crystal is combined to 4A molecular sieve |
| WO2020243770A1 (en) * | 2019-06-05 | 2020-12-10 | The University Of Queensland | Synthesis of adsorption materials |
| CN113924272A (en) * | 2019-06-05 | 2022-01-11 | 雷奥技术公司 | Synthesis of adsorbent Material |
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