CN104548954A - Hydrothermal synthesis method of SOD zeolite membrane - Google Patents
Hydrothermal synthesis method of SOD zeolite membrane Download PDFInfo
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- CN104548954A CN104548954A CN201310498695.6A CN201310498695A CN104548954A CN 104548954 A CN104548954 A CN 104548954A CN 201310498695 A CN201310498695 A CN 201310498695A CN 104548954 A CN104548954 A CN 104548954A
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- flyash
- hydrothermal synthesis
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Abstract
The invention relates to a hydrothermal synthesis method of an SOD zeolite membrane. The hydrothermal synthesis method comprises the following steps: roasting coal ash at the temperature of 800-850 DEG C for 2-6h, then soaking in a mixed solution of sulfuric acid and nitric acid for 16-30h, and uniformly grinding after drying; uniformly mixing the coal ash with silica solution, sodium hydroxide, sodium metaaluminate and deionized water in a proportion of coal ash, SiO2, Al2O3, NaAlO2 to H2O being (0.5-1.5g):(40-50 mol):(2-8 mol):(16-28 mol):(500-800 mol) to prepare crystallization mother liquid; putting a carrier in the crystallization mother liquid, and carrying out hydrothermal synthesis at the temperature of 80-120 DEG C for 6-15h; taking out after the reaction is completed, washing with deionized water, and drying at the temperature of 100 DEG C.
Description
Technical field
The invention belongs to inorganic material permeability and separation technical field, relate to a kind of preparation method of zeolite molecular sieve film, particularly a kind of hydrothermal synthesis method of SOD zeolite membrane.
Background technology
The cubic cell of SOD zeolite (sodalite) consists of Na
6[Al
6si
6o
24], its skeleton structure is by [SiO
4], [AlO
4] the sodalite cage that is interconnected of tetrahedron forms.Duct on the chemistry of zeolite molecular sieve film Yin Qigao and heat endurance, high mechanical strength, molecular dimension, tradable cation and can the solid acid/alkaline matter of modulation, have many application prospects in UF membrane, catalytic separation integration, functional material etc.Centrifugation is a critical function of zeolite membrane, and different because of structure composition, the character of zeolite membrane has hydrophily (or hydrophobicity).Usual zeolite membrane is all polycrystalline, and the existence of intracrystalline pore certainly will play an important role to separation process.
Fine cigarette ash under collecting from flue gas when flyash is coal-burning power plant's burning pulverized coal, belongs to pozzolanic materials.Containing a large amount of alumina silicate glass bodies in flyash, but wherein [SiO4]
4-the degree of polymerization is very high, compact structure, stable chemical nature, and its pozzolanic activity major part is potential, and slowly, this just greatly limit the exploitation of flyash to the speed of activation plays.At present, by the method for physics or chemistry, flyash, mainly for the preparation of zeolite molecular sieve, mineral polymeric material, devitrified glass, porous ceramics, compound catalyze material, also can be used as surrounding purifying material, polymer fill material, extraction SiO
2and Al
2o
3raw material etc.Synthesis zeolite is the field that fly ash development research on utilization relatively enlivens.Flyash is very similar to zeolite on composition, provides possibility for flyash changes into zeolite.Zeolite has that specific area is large, hydrothermal stability is high, micropore enriches equal first-class characteristic, can be widely used as the new function materials such as catalyst, adsorbent, ion-exchanger.The zeolite of flyash synthesis is mainly used to remove heavy metal ion in waste water, the ammonia of synchronous purification low concentration and phosphorus, process fluoride waste, the SO removed in useless underwater micro-organic matter and adsorbed gas in environment pollution control
2.
Summary of the invention
The object of the present invention is to provide a kind of hydrothermal synthesis method of SOD zeolite membrane.
The following technical scheme of concrete employing:
The hydrothermal synthesis method of SOD zeolite membrane, comprises the following steps:
1. flyash pretreatment: by flyash in 800 ~ 850 DEG C of roasting 2 ~ 6h, then 16 ~ 30h is soaked in the mixed solution of sulfuric acid and nitric acid, after dry, grinding is evenly;
2. crystallization mother liquor: flyash step 1. prepared and Ludox, NaOH, sodium metaaluminate and deionized water are by flyash: SiO
2: Al
2o
3: NaAlO
2: H
2o is that 0.5 ~ 1.5g:40 ~ 50mol:2 ~ 8mol:16 ~ 28mol:500 ~ 800mol mixes;
3. carrier is put into crystallization mother liquor 80 ~ 120 DEG C of Hydrothermal Synthesis 6 ~ 15h; React rear taking-up, spent deionized water, and dried at 100 DEG C.
The hydrothermal synthesis method of SOD zeolite membrane provided by the invention, described crystallization mother liquor presses proportioning flyash: SiO with flyash and Ludox, NaOH, sodium metaaluminate and deionized water
2: Al
2o
3: NaAlO
2: H
2o is 1g:40mol:4mol:20mol:800mol preparation.
The hydrothermal synthesis method of SOD zeolite membrane provided by the invention, described carrier is α-Al
2o
3pipe, mullite pipe or cordierite.
The hydrothermal synthesis method of SOD zeolite membrane provided by the invention, step is described flyash and 850 DEG C of roasting 2h 1., then soak 20h in the mixed solution of sulfuric acid and nitric acid.
The hydrothermal synthesis method of SOD zeolite membrane provided by the invention, the mixed solution of step 1. described sulfuric acid and nitric acid is sulfuric acid and the nitric acid mixed solution by concentration ratio 3mol/L:1mol/L.
The hydrothermal synthesis method of SOD zeolite membrane provided by the invention, described crystallization mother liquor is that NaOH, sodium metaaluminate is soluble in water, adds Ludox and stirs 10h, then adds flyash and stir 2h, forms stable crystallization mother liquor.
Compared to prior art, the present invention adopts the flyash after process to prepare crystallization mother liquor, can obtain the better SOD zeolite crystal of pattern, make the flyash discarded realize resource.And strengthen the mechanical strength of zeolite membrane, extend its service life.
Detailed description of the invention
The following examples can make the present invention of those of ordinary skill in the art's comprehend, but do not limit the present invention in any way.
Embodiment 1
The hydrothermal synthesis method of SOD zeolite membrane, comprises the following steps:
1. flyash pretreatment: by flyash in 800 DEG C of roasting 6h, then 16h is soaked in sulfuric acid and nitric acid are by the mixed solution of concentration ratio 3mol/L:1mol/L, after dry, grinding is evenly;
2. crystallization mother liquor: flyash step 1. prepared and Ludox, NaOH, sodium metaaluminate and deionized water are by flyash: SiO
2: Al
2o
3: NaAlO
2: H
2o is that 0.5g:40mol:2mol:16mol:500mol mixes;
3. carrier is put into crystallization mother liquor 80 DEG C of Hydrothermal Synthesis 15h; React rear taking-up, spent deionized water, and dried at 100 DEG C.
The hydrothermal synthesis method of the SOD zeolite membrane described in the present embodiment, described carrier is α-Al
2o
3pipe.
The hydrothermal synthesis method of the SOD zeolite membrane described in the present embodiment, described crystallization mother liquor is that NaOH, sodium metaaluminate is soluble in water, adds Ludox and stirs 10h, then adds flyash and stir 2h, forms stable crystallization mother liquor.
Embodiment 2
The hydrothermal synthesis method of SOD zeolite membrane, comprises the following steps:
1. flyash pretreatment: by flyash in 850 DEG C of roasting 2h, then 30h is soaked in sulfuric acid and nitric acid are by the mixed solution of concentration ratio 3mol/L:1mol/L, after dry, grinding is evenly;
2. crystallization mother liquor: flyash step 1. prepared and Ludox, NaOH, sodium metaaluminate and deionized water are by flyash: SiO
2: Al
2o
3: NaAlO
2: H
2o is that 1.5g:50mol:8mol:28mol:800mol mixes;
3. carrier is put into crystallization mother liquor 120 DEG C of Hydrothermal Synthesis 6h; React rear taking-up, spent deionized water, and dried at 100 DEG C.
The hydrothermal synthesis method of the SOD zeolite membrane described in the present embodiment, described carrier is mullite pipe.
The hydrothermal synthesis method of the SOD zeolite membrane described in the present embodiment, described crystallization mother liquor is that NaOH, sodium metaaluminate is soluble in water, adds Ludox and stirs 10h, then adds flyash and stir 2h, forms stable crystallization mother liquor.
Embodiment 3
The hydrothermal synthesis method of SOD zeolite membrane, comprises the following steps:
1. flyash pretreatment: by flyash in 850 DEG C of roastings 2, then 20h is soaked in sulfuric acid and nitric acid are by the mixed solution of concentration ratio 3mol/L:1mol/L, after dry, grinding is evenly;
2. crystallization mother liquor: flyash step 1. prepared and Ludox, NaOH, sodium metaaluminate and deionized water are by proportioning flyash: SiO
2: Al
2o
3: NaAlO
2: H
2o is 1g:40mol:4mol:20mol:800mol preparation.
3. carrier is put into crystallization mother liquor 80 ~ 120 DEG C of Hydrothermal Synthesis 6 ~ 15h; React rear taking-up, spent deionized water, and dried at 100 DEG C.
The hydrothermal synthesis method of the SOD zeolite membrane described in the present embodiment, described carrier is cordierite.
The hydrothermal synthesis method of the SOD zeolite membrane described in the present embodiment, described crystallization mother liquor is that NaOH, sodium metaaluminate is soluble in water, adds Ludox and stirs 10h, then adds flyash and stir 2h, forms stable crystallization mother liquor.
Claims (6)
- The hydrothermal synthesis method of 1.SOD zeolite membrane, comprises the following steps:1. flyash pretreatment: by flyash in 800 ~ 850 DEG C of roasting 2 ~ 6h, then 16 ~ 30h is soaked in the mixed solution of sulfuric acid and nitric acid, after dry, grinding is evenly;2. crystallization mother liquor: flyash step 1. prepared and Ludox, NaOH, sodium metaaluminate and deionized water are by flyash: SiO 2: Al 2o 3: NaAlO 2: H 2o is that 0.5 ~ 1.5g:40 ~ 50mol:2 ~ 8mol:16 ~ 28mol:500 ~ 800mol mixes;3. carrier is put into crystallization mother liquor 80 ~ 120 DEG C of Hydrothermal Synthesis 6 ~ 15h; React rear taking-up, spent deionized water, and dried at 100 DEG C.
- 2. the hydrothermal synthesis method of SOD zeolite membrane according to claim 1, is characterized in that: described crystallization mother liquor with flyash and Ludox, NaOH, sodium metaaluminate and deionized water by proportioning flyash: SiO 2: Al 2o 3: NaAlO 2: H 2o is 1g:40mol:4mol:20mol:800mol preparation.
- 3. the hydrothermal synthesis method of SOD zeolite membrane according to claim 1, is characterized in that: described carrier is α-Al 2o 3pipe, mullite pipe or cordierite.
- 4. the hydrothermal synthesis method of SOD zeolite membrane according to claim 1, is characterized in that: step is described flyash and 850 DEG C of roasting 2h 1., then soaks 20h in the mixed solution of sulfuric acid and nitric acid.
- 5. the hydrothermal synthesis method of the SOD zeolite membrane according to claim 1 or 3, is characterized in that: the mixed solution of step 1. described sulfuric acid and nitric acid is sulfuric acid and the nitric acid mixed solution by concentration ratio 3mol/L:1mol/L.
- 6. the hydrothermal synthesis method of SOD zeolite membrane according to claim 1, is characterized in that: described crystallization mother liquor is that NaOH, sodium metaaluminate is soluble in water, adds Ludox and stirs 10h, then adds flyash and stir 2h, forms stable crystallization mother liquor.
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|---|---|---|---|
| CN201310498695.6A CN104548954A (en) | 2013-10-21 | 2013-10-21 | Hydrothermal synthesis method of SOD zeolite membrane |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109012226A (en) * | 2018-07-27 | 2018-12-18 | 西安建筑科技大学 | A kind of application of ZSM-35 self-supporting molecular sieve film pervasion separation of heavy metal ions |
| CN110508159A (en) * | 2019-08-16 | 2019-11-29 | 南方科技大学 | Zeolite nano-filtration membrane and preparation method thereof |
-
2013
- 2013-10-21 CN CN201310498695.6A patent/CN104548954A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109012226A (en) * | 2018-07-27 | 2018-12-18 | 西安建筑科技大学 | A kind of application of ZSM-35 self-supporting molecular sieve film pervasion separation of heavy metal ions |
| CN109012226B (en) * | 2018-07-27 | 2021-03-26 | 西安建筑科技大学 | Application of ZSM-35 self-supporting molecular sieve membrane in permeation separation of heavy metal ions |
| CN110508159A (en) * | 2019-08-16 | 2019-11-29 | 南方科技大学 | Zeolite nano-filtration membrane and preparation method thereof |
| CN110508159B (en) * | 2019-08-16 | 2022-04-29 | 南方科技大学 | Zeolite nanofiltration membrane and process for preparing the same |
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Application publication date: 20150429 |