CN104548955A - Microwave synthesis method of SOD zeolite membrane - Google Patents
Microwave synthesis method of SOD zeolite membrane Download PDFInfo
- Publication number
- CN104548955A CN104548955A CN201310500381.5A CN201310500381A CN104548955A CN 104548955 A CN104548955 A CN 104548955A CN 201310500381 A CN201310500381 A CN 201310500381A CN 104548955 A CN104548955 A CN 104548955A
- Authority
- CN
- China
- Prior art keywords
- flyash
- zeolite membrane
- crystallization mother
- synthesizing
- mother liquor
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The invention relates to a microwave synthesis method of an SOD zeolite membrane. The microwave 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 microwave synthesis at the temperature of 80-120 DEG C for 2-8h; taking out after the reaction is completed, and supplementing the same amount of crystallization mother liquid at the temperature of 50-80 DEG C to carry out microwave synthesis for 0-4h; 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 microwave process for synthesizing of SOD zeolite membrane.
Background technology
Microwave is a kind of high frequency electromagnetic radiation with 0.3 ~ 3GHz.Microwave technology is widely used in each research field, as biology and medical science etc.After the eighties, microwave technology starts to be applied to chemical field, and starts in the nineties synthesis being applied to zeolite.Compared with traditional hydrothermal synthesis method, it is short that microwave heating method has generated time, dynamics narrowly distributing, widely synthetic ingredient and highly purified advantage.These advantages promote scientists and explore its application widely in synthesizing molecular sieve film.
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 microwave process for synthesizing of SOD zeolite membrane.
The following technical scheme of concrete employing:
The microwave process for synthesizing 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 Microwave synthesize 2 ~ 8h; React rear taking-up, supplement crystallization mother liquor 50 ~ 80 DEG C of Microwave synthesize 0 ~ 4h of identical amount; Spend deionized water, and dry at 100 DEG C.
The microwave process for synthesizing 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 microwave process for synthesizing of SOD zeolite membrane provided by the invention, described carrier is α-Al
2o
3pipe, mullite pipe or cordierite.
The microwave process for synthesizing 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 microwave process for synthesizing 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:2mol/L.
The microwave process for synthesizing 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 preparation crystallization mother liquor after process, 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.Microwave process for synthesizing can shorten film formation time.
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 microwave process for synthesizing 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:2mol/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:50mol:2mol:28mol:5000mol mixes;
3. carrier is put into crystallization mother liquor 120 DEG C of Microwave synthesize 2h; React rear taking-up, supplement crystallization mother liquor 80 DEG C of Microwave synthesize 4h of identical amount; Spend deionized water, and dry at 100 DEG C.
The microwave process for synthesizing of the SOD zeolite membrane described in the present embodiment, described carrier is α-Al
2o
3pipe.
The microwave process for synthesizing 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 microwave process for synthesizing 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:2mol/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:40mol:8mol:16mol:800mol mixes;
3. carrier is put into crystallization mother liquor 80 DEG C of Microwave synthesize 8h; React rear taking-up; Spend deionized water, and dry at 100 DEG C.
The microwave process for synthesizing of the SOD zeolite membrane described in the present embodiment, described carrier is mullite pipe.
The microwave process for synthesizing 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 microwave process for synthesizing of SOD zeolite membrane, comprises the following steps:
1. flyash pretreatment: by flyash in 850 DEG C of roasting 2h, then 20h is soaked in sulfuric acid and nitric acid are by the mixed solution of concentration ratio 3mol/L:2mol/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 1g:40mol:4mol:20mol:800mol mixes;
3. carrier is put into crystallization mother liquor 100 DEG C of Microwave synthesize 4h; React rear taking-up, supplement crystallization mother liquor 60 DEG C of Microwave synthesize 2h of identical amount; Spend deionized water, and dry at 100 DEG C.
The microwave process for synthesizing of SOD zeolite membrane provided by the invention, described carrier is cordierite.
The microwave process for synthesizing 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.
Claims (6)
- The microwave process for synthesizing 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 Microwave synthesize 2 ~ 8h; React rear taking-up, supplement crystallization mother liquor 50 ~ 80 DEG C of Microwave synthesize 0 ~ 4h of identical amount; Spend deionized water, and dry at 100 DEG C.
- 2. the microwave process for synthesizing 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 microwave process for synthesizing 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 microwave process for synthesizing 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 microwave process for synthesizing 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:2mol/L.
- 6. the microwave process for synthesizing 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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310500381.5A CN104548955A (en) | 2013-10-21 | 2013-10-21 | Microwave synthesis method of SOD zeolite membrane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310500381.5A CN104548955A (en) | 2013-10-21 | 2013-10-21 | Microwave synthesis method of SOD zeolite membrane |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104548955A true CN104548955A (en) | 2015-04-29 |
Family
ID=53066668
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310500381.5A Pending CN104548955A (en) | 2013-10-21 | 2013-10-21 | Microwave synthesis method of SOD zeolite membrane |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104548955A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105214608A (en) * | 2015-09-23 | 2016-01-06 | 哈尔滨理工大学 | Coal ash for manufacturing is for the method without templet of petal-shaped sodalite and white carbon composite balls bunch |
-
2013
- 2013-10-21 CN CN201310500381.5A patent/CN104548955A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105214608A (en) * | 2015-09-23 | 2016-01-06 | 哈尔滨理工大学 | Coal ash for manufacturing is for the method without templet of petal-shaped sodalite and white carbon composite balls bunch |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Ren et al. | Synthesis of zeolites from coal fly ash for the removal of harmful gaseous pollutants: A review | |
| CN101618869B (en) | Method for preparing small-size meso-porous hollow carbon sphere | |
| CN103769045B (en) | A kind of preparation method of fly ash base high-performance adsorbing material | |
| CN104525090A (en) | Absorbent used in sewage phosphorus removal, and preparation method thereof | |
| CN103394367A (en) | Preparation method of ZSM-5 molecular sieve core shell double-layer catalyst by utilizing fly ash | |
| CN105833899A (en) | Preparation method for SCR catalyst for purifying oxynitride in motor vehicle exhaust | |
| CN104437355A (en) | Preparation method of coal ash-based CuO-CeO2/FAU desulfurizer | |
| WO2011127737A1 (en) | Modified molecular sieve with high selectivity to ammonia nitrogen in waste water and preparation method thereof | |
| CN111659251A (en) | Low-cost hierarchical pore SAPO-34 molecular sieve and preparation method and application thereof | |
| CN111905690A (en) | Method for preparing water body nitrogen and phosphorus removal oxygenation composite material by utilizing coal ash | |
| CN108622904A (en) | The method of mesoporous microballon and mesoporous microballon obtained are prepared using coal gasification fine slag | |
| CN107746065A (en) | A kind of method for preparing the molecular screen membrane of high-performance SAPO 34 | |
| CN102795631B (en) | Method for preparing silicon dioxide aerogel | |
| CN104692410A (en) | Method for synthesizing A molecular sieve by crystallizing wet gel | |
| CN104492475A (en) | Preparation method of micropore-mesopore ZSM-5/Pd-gamma-Al2O3 composite catalyst | |
| CN112191221A (en) | Adsorbent for rapidly and efficiently removing nitrogen and phosphorus and preparation method thereof | |
| CN113548673B (en) | Method for preparing molecular sieve by using lithium slag | |
| CN104190464A (en) | Preparation method of Sn-based micropore molecular sieve NOx-SCR (selective catalytic reduction) catalyst | |
| CN104548954A (en) | Hydrothermal synthesis method of SOD zeolite membrane | |
| CN109433217A (en) | A kind of red mud denitrating catalyst and preparation method thereof | |
| CN104548955A (en) | Microwave synthesis method of SOD zeolite membrane | |
| US10570065B1 (en) | Method of fabricating green desiccant wheel | |
| CN104028219A (en) | Method for preparing activated carbon-4A type molecular sieve composite material by utilizing coal gangue | |
| CN115385356A (en) | Method for preparing 13X molecular sieve by using fly ash solid phase | |
| CN104129924B (en) | A kind of preparation method of the opal glass coating with photocatalysis performance |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20150429 |
|
| WD01 | Invention patent application deemed withdrawn after publication |