CN105800643A - Method for preparing 13X molecular sieve by cooperation of coal gangue and coal ash desilication liquid - Google Patents
Method for preparing 13X molecular sieve by cooperation of coal gangue and coal ash desilication liquid Download PDFInfo
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- CN105800643A CN105800643A CN201610127420.5A CN201610127420A CN105800643A CN 105800643 A CN105800643 A CN 105800643A CN 201610127420 A CN201610127420 A CN 201610127420A CN 105800643 A CN105800643 A CN 105800643A
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- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
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Abstract
The invention discloses a method for preparing a 13X molecular sieve by cooperation of coal gangue and a coal ash desilication liquid. The method comprises the following processing steps: crushing, grinding and screening coal gangue, carrying out high-temperature calcination and activating pretreatment; carrying out wet-milling, mixing wet-milled slurry with the coal ash desilication liquid as an aluminum source and partial silicon source; and carrying out ageing, crystallizing, filtering, washing and drying in an alkaline environment to prepare the 13X molecular sieve. By the preparation method of the 13X molecular sieve, the production cost of the 13X molecular sieve is reduced; the resource utilization rate of the coal gangue is improved; an effective utilization way of the coal ash desilication liquid with high alkaline content and low modulus is expanded; integration of alkaline liquid recovery and industrial waste resource recycling processes is achieved; environmental protection is facilitated; and the method is a clean circulating production technology.
Description
Technical field
The invention belongs to coal measures trade waste higher value application technical field, be specifically related to a kind of method preparing 13X molecular sieve for the collaborative flyash desiliconization liquid of raw material with gangue.
Background technology
Gangue is and the rock of coal association, is the solid waste being separated in coal mining and dressing of coal by washing process, accounts for more than the 40% of China's industrial solid castoff discharge capacity.Soil, air and water body all can be caused serious pollution by gangue air storage.Therefore, carry out utilization of coal gangue and utilize particularly important, SiO in gangue2And Al2O3Content about 70%～90%, utilizes gangue component characteristic, it is possible to as the raw material preparing aluminum silicon system molecular sieve.
Molecular sieve is a kind of to have connected pore channel, moisture aluminosilicate compound in skeleton structure shape.Special structure is so as to have the excellent properties such as ion exchange, efficient selective absorption, catalysis, and therefore molecular screen material has become the focus of research.Wherein 13X molecular sieve is the larger-size molecular sieve of opposite cell (0.9nm), is widely used in gas separation, CO2The field such as pressure-variable adsorption, space division, demand is big.And tradition chemical industry production cost is higher; ingredient requirement is strict; therefore prepare 13X molecular sieve with gangue to be possible not only to reduce 13X Zeolite synthesis cost; the value of resource can also be improved; turn waste into wealth; alleviate gangue and cause the pressure of environmental pollution, protect environment, meet basic principle high-valued, recycling.
In recent years, the method that gangue prepares 13X molecular sieve is utilized to include: Tian Zhen etc. utilize gangue to add the Hydrothermal Synthesis 13X molecular sieves such as part silicon source such as waterglass, Ludox, white carbon；Kong Deshun etc. utilize Coaseries kaolin to add the test of sodium silicate Hydrothermal Synthesis 13X molecular sieve；CN104556119A report Huang Ling coal slime is prepared interpolation hydrochloric acid removing part aluminium oxide in 13X molecular sieve process and is reached to meet the silica alumina ratio of 13X Zeolite synthesis.But, synthesizing 13X molecular sieve with gangue in said method needs interpolation chemical raw material to cause synthesis relatively costly, or extraction part aluminium oxide causes complex process.And aluminous fly-ash preparing mullite or extract alumina resource can the substantial amounts of high alkalinity desiliconization liquid of by-product, desiliconization liquid is richly stored with silicon resource and sodium resource.Therefore, this patent proposes to prepare 13X molecular sieve with the collaborative flyash desiliconization liquid of gangue, is that dissolving on a large scale of two kinds of garbages finds effective way, it is achieved the purpose of solid waste resource higher value application.
Summary of the invention
It is an object of the invention to provide a kind of method preparing 13X molecular sieve with the collaborative flyash desiliconization liquid of gangue.According to the compositing characteristic that flyash desiliconization liquid modulus is relatively low, using gangue as aluminum source and part silicon source, using desiliconization liquid as the silicon source of sodium source and another part, hydrothermal synthesis method is adopted to prepare 13X molecular sieve.Improve utilization of coal gangue utilization rate; expand the Processes For Effective Conversion of the flyash desiliconization liquid that alkalinity is high, modulus is low; achieve recycle of alkali liquor and utilize the integrated of process, environmentally friendly protection with trade waste resource recycling, be a kind of cleaning cycle production process.
For reaching this purpose, the present invention by the following technical solutions:
(1) gangue pretreatment: be ground by gangue, sieve, calcining and activating processes；
(2) gangue wet ground: activating coal gangue powder and water are by 1:(0.5～10) carry out wet grinding, the wet grinding time is 10～180min, prepares gangue slip；
(3) ripening: gangue slip step (2) prepared is allocated according to the mol ratio of oxide with flyash desiliconization liquid, n (SiO2/Al2O3)=2.6～3.6, n (Na2O/SiO2)=1.5～2.5, n (H2O/Na2O)=30～80, heating, to 30～60 DEG C, is stirred mixing 10～80min, is cooled to room temperature ageing 0～36h；
(4) Crystallizing treatment: ageing slip Crystallizing treatment step 3 prepared, crystallization temperature 70～120 DEG C, crystallization time 4～14h, crystal pattern stands or stirring, adds crystal seed 1～10wt%.It is 9～11 by the slurry filtration after crystallization, washing to the pH of filtrate, dry obtains described 13X molecular sieve at 60～140 DEG C.
Described in step (1), gangue adopts ball mill to carry out ball milling, and Ball-milling Time is 30～120min, is milled to 100～600 orders, and calcining heat is 700～1000 DEG C, and calcination time is 2～8h.
Flyash desiliconization liquid described in step (3) be mainly composed of sodium hydroxide and sodium silicate, the Na ion concentration of described sodium hydroxide is 20-200g/L, and the atom concentration of described sodium silicate is 10-100g/L.
The liquid that solid-liquid separation described in step (4) obtains is mainly sodium hydroxide solution, it is possible to returns and continues desiliconization, reaches the effect that alkali liquor recycles.
Compared with prior art, it is an advantage of the current invention that: provide a kind of method utilizing the collaborative flyash desiliconization liquid of gangue to prepare 13X molecular sieve, not only expand the source of 13X Zeolite synthesis raw material, additionally provide the Processes For Effective Conversion of the flyash desiliconization liquid that a kind of alkali content is high, modulus is low, turn waste into wealth.And this preparation method is simple, and reaction condition is controlled, and equipment requirements is not high.13X molecular sieve cost is greatly lowered, and can realize again alkali liquor and recycle integrated with trade waste recycling process.
Illustrate that the present invention is described in more detail with embodiment below in conjunction with accompanying drawing.
Accompanying drawing explanation
Fig. 1 is the process chart utilizing the collaborative flyash desiliconization liquid of gangue to prepare 13X molecular sieve provided by the invention.
Fig. 2 is the XRD spectra of the 13X molecular sieve of the embodiment of the present invention 1 preparation.
Detailed description of the invention
Specific embodiment disclosed in this invention and method, its description is exemplary rather than restrictive.
Embodiment 1
With abrading-ball and gangue mass ratio for 2:1, ball milling 30min, select the gangue of 200～325 orders, 800 DEG C of calcining 8h, obtain activating coal gangue powder.Activating coal gangue powder and water carry out wet grinding, wet grinding 30min by 1:3, obtain slip.Then according to allocate according to the mol ratio of oxide, n (SiO2/Al2O3)=3.0, n (Na2O/SiO2)=1.7, n (H2O/Na2O)=60, with flyash desiliconization liquid at 55 DEG C, stirring 60min under 100 revs/min of conditions of speed of agitator, it is cooled to room temperature ageing 24h.By ageing slip at 90 DEG C, seed load 1%wt, crystallization 8h under 100 revs/min of conditions of speed of agitator, product filters, and adds water washing 2 times, and 80 DEG C of dry 24h obtain CO2Adsorption rate 23.4%, specific surface area 681.7m2/ g, relative crystallinity 94.59% 13X molecular sieve.
Embodiment 2
With abrading-ball and gangue mass ratio for 1:1, ball milling 40min, select the gangue of 200～325 orders, 850 DEG C of calcining 6h, obtain activating coal gangue powder.Activating coal gangue powder and water carry out wet grinding, wet grinding 10min by 1:0.5, obtain slip.Then according to allocate according to the mol ratio of oxide, n (SiO2/Al2O3)=3.4, n (Na2O/SiO2)=1.7, n (H2O/Na2O)=40, with flyash desiliconization liquid at 55 DEG C, stirring 50min under 200 revs/min of conditions of speed of agitator, it is cooled to room temperature ageing 14h.By ageing slip at 100 DEG C, seed load 5wt, crystallization 10h under 100 revs/min of conditions of speed of agitator, product filters, and adds water washing 3 times, and 100 DEG C of dry 16h obtain CO2Adsorption rate 19.8%, specific surface area 540m2/ g, relative crystallinity 79.93% 13X molecular sieve.
Embodiment 3
With abrading-ball and gangue mass ratio for 3:1, ball milling 50min, select the gangue of 200～325 orders, 850 DEG C of calcining 5h, obtain activating coal gangue powder.Activating coal gangue powder and water press 1:5 row wet grinding, wet grinding 90min, obtain slip.Then according to allocate according to the mol ratio of oxide, n (SiO2/Al2O3)=3.0, n (Na2O/SiO2)=1.8, n (H2O/Na2O)=50, with flyash desiliconization liquid at 55 DEG C, stirring 30min under 200 revs/min of conditions of speed of agitator, it is cooled to room temperature ageing 20h.By ageing slip 95, crystallization 8h under seed load 7%wt, 300 revs/min of conditions of speed of agitator, product filters, and adds water washing 3 times, and 120 DEG C of dry 12h obtain CO2Adsorption rate 22.0%, specific surface area 665.8m2/ g, relative crystallinity 93.65% 13X molecular sieve.
Embodiment 4
With abrading-ball and gangue mass ratio for 2:1, ball milling 60min, select the gangue of 200～325 orders, 900 DEG C of calcining 4h, obtain activating coal gangue powder.Activating coal gangue powder and water carry out wet grinding, wet grinding 120min by 1:7, obtain slip.Then according to allocate according to the mol ratio of oxide, n (SiO2/Al2O3)=3.2, n (Na2O/SiO2)=1.9, n (H2O/Na2O)=50, with flyash desiliconization liquid at 55 DEG C, stirring 30min under 200 revs/min of conditions of speed of agitator, it is cooled to room temperature ageing 24h.By ageing slip at 100 DEG C, seed load 3%wt, crystallization 8h under 400 revs/min of conditions of speed of agitator, product filters, and adds water washing 3 times, and 120 DEG C of dry 12h obtain CO2Adsorption rate 22.6%, specific surface area 622.4m2/ g, relative crystallinity 87.63% 13X molecular sieve.
Embodiment 5
With abrading-ball and gangue mass ratio for 1:1, ball milling 40min, select the gangue of 200～325 orders, 950 DEG C of calcining 2h, obtain activating coal gangue powder.Activating coal gangue powder and water carry out wet grinding, wet grinding 180min by 1:10, obtain slip.Then according to allocate according to the mol ratio of oxide, n (SiO2/Al2O3)=2.8, n (Na2O/SiO2)=2.1, n (H2O/Na2O)=60, with flyash desiliconization liquid at 55 DEG C, stirring 20min under 200 revs/min of conditions of speed of agitator, it is cooled to room temperature ageing 18h.By ageing slip at 90 DEG C, seed load 1%wt, crystallization 8h under 400 revs/min of conditions of speed of agitator, product filters, and adds water washing 4 times, and 80 DEG C of dry 24h obtain CO2Adsorption rate 18.6%, specific surface area 603.7m2/ g, relative crystallinity 86.24% 13X molecular sieve.
Non-elaborated part of the present invention belongs to the known technology of those skilled in the art.
Applicant states, the present invention illustrates the method detailed of the present invention by above-described embodiment, but the invention is not limited in above-mentioned method detailed, does not namely mean that the present invention has to rely on above-mentioned method detailed and could implement.The equivalence of each raw material of product of the present invention, it will be clearly understood that any improvement in the present invention, is replaced and the interpolation of auxiliary element, concrete way choice etc. by person of ordinary skill in the field, all falls within protection scope of the present invention and open scope.
Claims (4)
1. one kind utilizes the method that the collaborative flyash desiliconization liquid of gangue prepares 13X molecular sieve, it is characterised in that:
(1) gangue pretreatment: be ground by gangue, sieve, calcining and activating processes, and obtains activating coal gangue powder；
(2) gangue wet ground: activating coal gangue powder step (1) obtained and water carry out wet grinding and prepares gangue slip；
(3) ripening: gangue slip step (2) prepared carries out ageing reaction after stirring in proportion with flyash desiliconization liquid, prepares ageing slip；
(4) Crystallizing treatment: ageing slip step (3) obtained at high temperature carries out crystallization, obtains solidliquid mixture, is easily separated by solidliquid mixture, gained solid phase obtains 13X molecular sieve through washing, drying.
2. method according to claim 1, it is characterised in that: described in step (1), in gangue, silica alumina ratio is 1.6～2.5, and ball milling particle diameter is 100～600 orders；Calcined coal gangue temperature is 700～1000 DEG C, and calcination time is 2～8h.
3. method according to claim 1, it is characterised in that: described in step (2), the preparation of gangue slip according to activating coal gangue powder and water with mass ratio 1:(0.5～10) carry out wet grinding, wet grinding time 10mim～180min.
4. method according to claim 1, it is characterised in that: described in step (3), the Na ion concentration in flyash desiliconization liquid is 20-200g/L, and atom concentration is 10-100g/L.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106587098A (en) * | 2016-12-01 | 2017-04-26 | 神华集团有限责任公司 | Method for extracting aluminum residues to prepare 13X type molecular sieve and ZSM-5 type molecular sieve through pulverized fuel ash acid method and using method of pulverized fuel ash |
| CN108190904A (en) * | 2017-12-19 | 2018-06-22 | 华电电力科学研究院 | A kind of method and performance test methods that molecular sieve sorbing material is prepared with the direct alkali fusion-hydro-thermal method of high-calcium fly ass |
| CN110314642A (en) * | 2019-05-28 | 2019-10-11 | 昌鑫生态科技(陕西)有限公司 | Industrial Solid Waste processes high-performance adsorbent material production technology |
| CN113353949A (en) * | 2021-06-30 | 2021-09-07 | 东北大学 | Synthetic zeolite of fly ash and coal gangue aluminum extraction slag and comprehensive utilization method thereof |
| CN113401917A (en) * | 2021-07-07 | 2021-09-17 | 北京科技大学 | Preparation method for synthesizing pure-phase P-type molecular sieve by using activated fly ash silicon-aluminum insoluble phase |
| CN113428874A (en) * | 2021-05-31 | 2021-09-24 | 东南大学 | Preparation method and application method of gangue-based sodium ion type molecular sieve based on alkali fusion method |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106587098A (en) * | 2016-12-01 | 2017-04-26 | 神华集团有限责任公司 | Method for extracting aluminum residues to prepare 13X type molecular sieve and ZSM-5 type molecular sieve through pulverized fuel ash acid method and using method of pulverized fuel ash |
| CN108190904A (en) * | 2017-12-19 | 2018-06-22 | 华电电力科学研究院 | A kind of method and performance test methods that molecular sieve sorbing material is prepared with the direct alkali fusion-hydro-thermal method of high-calcium fly ass |
| CN110314642A (en) * | 2019-05-28 | 2019-10-11 | 昌鑫生态科技(陕西)有限公司 | Industrial Solid Waste processes high-performance adsorbent material production technology |
| CN113428874A (en) * | 2021-05-31 | 2021-09-24 | 东南大学 | Preparation method and application method of gangue-based sodium ion type molecular sieve based on alkali fusion method |
| CN113353949A (en) * | 2021-06-30 | 2021-09-07 | 东北大学 | Synthetic zeolite of fly ash and coal gangue aluminum extraction slag and comprehensive utilization method thereof |
| CN113401917A (en) * | 2021-07-07 | 2021-09-17 | 北京科技大学 | Preparation method for synthesizing pure-phase P-type molecular sieve by using activated fly ash silicon-aluminum insoluble phase |
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