CN106865565A - A kind of flyash synthesizes the method for X-type zeolite - Google Patents

A kind of flyash synthesizes the method for X-type zeolite Download PDF

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CN106865565A
CN106865565A CN201710185726.0A CN201710185726A CN106865565A CN 106865565 A CN106865565 A CN 106865565A CN 201710185726 A CN201710185726 A CN 201710185726A CN 106865565 A CN106865565 A CN 106865565A
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flyash
type zeolite
reaction kettle
calcining
zeolite
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刘勇
王璐
王国栋
李现龙
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Tianjin University
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B39/00Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
    • C01B39/02Crystalline 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
    • C01B39/20Faujasite type, e.g. type X or Y
    • C01B39/22Type X
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/80Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/82Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/80Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/88Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by thermal analysis data, e.g. TGA, DTA, DSC
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/03Particle morphology depicted by an image obtained by SEM
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/12Surface area

Abstract

The present invention relates to a kind of method that flyash synthesizes X-type zeolite;The calcining of 100 200 mesh raw material flyash is obtained except the raw material after carbon;By the coal-ash immersion after calcining in hydrochloric acid solution, stirring reaction, then filtering, filter cake is washed to pH=6.0 7.0, is then placed in oven drying;Plus sodium metasilicate, NaOH and distilled water, mixed material, ageing is stirred at room temperature;It is then transferred in hydrothermal reaction kettle, seals, then hydrothermal reaction kettle is put into baking oven, is reacted at 90 105 DEG C;After the completion of reaction, hydrothermal reaction kettle is taken out, be cooled to room temperature, filter solid product, and filter cake is washed with distilled water, until wash solution pH to 8.5 10, is put into oven drying after filtering, obtain X-type zeolite.X-type zeolite is three-dimensional octahedral structure, and crystal formation is clear-cut, and form is intact, uniform particle diameter;Its TG-DT A spectrum illustrates X-type zeolite good thermal stability.

Description

A kind of flyash synthesizes the method for X-type zeolite
Technical field
The silicon in the flyash that generation is discharged after coal burns, the method that silicon source prepares X-type zeolite are the present invention relates to the use of, Specifically, it is a kind of method of flyash synthesis X-type zeolite;Belong to Solid Waste Treatment and resource field.
Background technology
Coal is the energy core of China's industrial development, as thermal power plant largely uses coal, and coal in China ash Divide higher, trade waste flyash yield that is coal-fired and producing is increased sharply, but utilization rate is increasesd slowly, and flyash is entered Row landfill disposal not only wastes a large amount of land resources, but also pollutes environment.At present, the recycling of flyash is mainly being built The fields such as building materials, chemical industry, environmental protection, agricultural are built, building trade field accounts for the 30% of total amount.Due to containing titanium dioxide in flyash Silicon and aluminum oxide, it is similar to zeolite main component, the zeolite molecular sieve of high added value is synthesized using flyash.Using flyash The zeolite molecular sieve of synthesis processes heavy metal-containing waste water, can not only improve the added value of flyash, while being also containing heavy metal The improvement of waste water so not only reaches the effect of the treatment of wastes with processes of wastes against one another, and also function to money there is provided a kind of processing method of low cost The effect that source utilizes.
X-type zeolite is a kind of nanomicroporous material, with preferably absorption, catalysis and the performance such as ion exchange, chemical industry, It is widely used in the field such as environmental protection and medical and health and huge market potential.Artificial synthesized X-type zeolite with Natural faujasite has identical crystal structure, and silica alumina ratio is less than 1.5.X-type zeolite molecular sieve belongs to cubic system, its reason The structure cell thought is constituted:Na86(Al86Si106O384)·264H20, cell parameter α are 2.486-2.502nm, and space group is Fd3m, Each structural units of X-type molecular sieve has 192 silicon (aluminium) oxygen tetrahedrons to constitute, and effective aperture is 0.9-1.0nm.This knot Structure can provide quick micropore diffusion advantage for suction-operated, effectively improve adsorption capacity.
Zeolite is a kind of widely used inorganic porous material, extensive due to its special architectural feature and performance It is applied to effluent containing heavy metal ions treatment, exhaust-gas treatment, separation and the industrial circle such as drying and oil catalysis of gas.Naturally Zeolite is influenceed by region and mining conditions, can not fully meet the industrial demand to amount of zeolite.Although zeolite can be carried out It is artificial synthesized, but utilize pure industrial chemicals synthetic zeolite relatively costly, equally also limit zeolite answering in low side field With.At present, X-type zeolite is mainly using caustic soda, aluminium hydroxide, waterglass etc. as raw material, using the technique of low-temperature hydrothermal synthesis Production.But because synthesis technique does not have important breakthrough, synthesized X-type zeolite product purity is not high, the low reason of yield, profit The industrial problems for synthesizing X-type zeolite with raw mineral materials are not solved still so far.Find suitable inexpensive raw material turn into solve this The key of one problem.Due to containing silica and aluminum oxide in flyash, the main component to zeolite is similar, so using powder Coal ash synthesis X-type zeolite has good prospect.
The content of the invention
Can be improvement and the resource profit of flyash it is an object of the invention to provide the method that flyash synthesizes X-type zeolite With the offer choice of technology.
Technical scheme is as follows:
A kind of flyash synthesizes the method for X-type zeolite, and its step is as follows:
1) 100-200 mesh raw materials flyash is calcined, is obtained except the raw material after carbon;
2) by the coal-ash immersion after calcining in hydrochloric acid solution, stirring reaction, then filtering, filter cake is washed to pH= 6.0-7.0, is then placed in oven drying;
3) to step 2) treatment after flyash in plus sodium metasilicate, NaOH and distilled water, mixed material, at room temperature Stirring ageing;It is then transferred in hydrothermal reaction kettle, seals, then hydrothermal reaction kettle is put into baking oven, it is anti-at 90-105 DEG C Should;After the completion of reaction, hydrothermal reaction kettle is taken out, be cooled to room temperature, filter solid product, and filter cake is washed with distilled water Wash, until wash solution pH to 8.5-10, is put into oven drying after filtering, obtain X-type zeolite.
Preferred steps 1) calcining heat be 550-850 DEG C, calcination time is 2-4h.
Preferred steps 2) in, in the hydrochloric acid solution of 3.5-4.5mol/L, solid-to-liquid ratio is used the coal-ash immersion after calcining 1:9~11 (g/ml).
Preferred steps 2) at 90 DEG C stirring reaction 4-5h.
Preferred steps 3) digestion time be 10-12h.
Preferred steps 3) material ratio is respectively:Sodium metasilicate and step 2) the flyash quality ratio that obtains is 1~2.5:1, hydrogen Sodium oxide molybdena and step 2) the flyash quality ratio that obtains is fixed as 0.58:1, distilled water volume and flyash and sodium silicate mixture The quality of material is 5.0~10 than scope:1.
Preferred steps 3) reaction time be 8-24h.
It is preferred that oven drying temperature is 105 DEG C
The present invention obtains a kind of method that flyash synthesizes X-type zeolite;Scanning electron microscopic observation X-type zeolite is three-dimensional octahedra Structure, crystal formation is clear-cut, and form is intact, uniform particle diameter;X-type zeolite product chemical formula is:Si7Al5O24Na7.4(H2O)5.2, With PDF standard card PDF#83-2319, powder x-ray diffraction figure characteristic peak angle of diffraction (2 θ) value is 6.080 °, 9.997 °, 12.380°、15.461°、17.618°、20.763°、21.580°、23.360°、26.559°、28.021°、33.757°、 35.600 °, the scanning electron microscope (SEM) photograph and powder x-ray diffraction figure of the X-type zeolite of synthesis are as shown in Figure 1 and Figure 2.Infrared spectrogram ripple Position long is close with X-type zeolite infrared spectrogram in document, can be further characterized by synthetic product for X-type zeolite, its infrared spectrum Figure is as shown in Figure 5;TG-DTA analysis illustrate X-type zeolite good thermal stability.
It is described as follows:
Milled processed:Raw material flyash is ground using comminuted grinder, with this as synthetic zeolite raw material; The purpose of this step is to reduce grain graininess, and is more uniformly distributed solid particle, is more beneficial for subsequent reactions.
High-temperature calcination:Take the flyash after grinding to be placed in crucible, the high-temperature calcination 2-4h at 550-850 DEG C of Muffle furnace, The carbon of uncombusted in flyash is removed, flyash is changed into yellow by grey after calcining.
The molten treatment of acid:In the hydrochloric acid solution of 3.4-4.5mol/L, solid-to-liquid ratio uses 1 to coal-ash immersion after calcining:9~ 11 (mass/volume, g/ml), stirring reaction 4-5h at 90 DEG C, then filtering, filter cake are washed to neutrality, are then done at 105 DEG C It is dry;The purpose of pickling is to remove some impurity in flyash, such as iron, calcium, sodium, sulphur soluble impurity, after being conducive to improving The purity of continuous synthetic zeolite.
Hydrothermal Synthesiss:Then exist to sodium metasilicate, NaOH and distilled water, mixed material is added in the flyash after treatment Stirring ageing 10-12h, is then transferred in hydrothermal reaction kettle at room temperature, seals, then hydrothermal reaction kettle is put into baking oven, 8-24h is reacted at 90-105 DEG C.After the completion of reaction, hydrothermal reaction kettle is taken out, be cooled to room temperature, outwell supernatant, cross filter solid Product, and filter cake is washed with distilled water, until wash solution pH to 8.5-10, is put into baking oven after filtering, at 105 DEG C Fully dry, you can obtain X-type zeolite.
The invention provides one kind conveniently, the method for succinct, easily operated Hydrothermal Synthesiss X-type zeolite.The X-type boiling of synthesis Stone product crystal formation is intact, and in octahedral structure, powder x-ray diffraction figure (XRD) characteristic peak is clearly intact.Normal temperature to 200 DEG C it Between there is obvious weightlessness, there is endothermic peak in its DSC data, mainly due to zeolite adsorption moisture and partially crystallizable water Overflow, slow weightlessness is still present between 200 DEG C to 700 DEG C, and DSC data shows to be deposited between 350 DEG C to 700 DEG C May be still, because the substep dehydration of the partially crystallizable moisture in X-type zeolite causes, also may be used at more heat absorption fluctuation peak Can there is crystal structure breakoff phenomenon, the thermogravimetric of the X-type zeolite of synthesis, derivative thermogravimetric analysis figure and Differential Scanning Calorimetry analysis chart As shown in Figure 3, Figure 4.The X-type zeolite has good heat endurance.Its infrared spectrum is close with pure X-type zeolite.BET methods are surveyed The X-type zeolite specific surface area for obtaining is 133m2/g。
Brief description of the drawings
Fig. 1:105 DEG C of crystallization synthesize the scanning electron microscope (SEM) photograph of X-type zeolite;
Fig. 2:Synthesize the powder x-ray diffraction figure of X-type zeolite;
Fig. 3:Synthesize thermogravimetric, the derivative thermogravimetric analysis figure of X-type zeolite;
Fig. 4:Synthesize the Differential Scanning Calorimetry analysis chart of X-type zeolite;
Fig. 5:Synthesize the infrared spectrogram of X-type zeolite;
Fig. 6:Crystallization synthesizes the scanning electron microscope (SEM) photograph of X-type zeolite at 95 DEG C;
Fig. 7:8h crystallization synthesizes the powder x-ray diffraction figure of X-type zeolite at 95 DEG C;
Fig. 8:12h crystallization synthesizes the powder x-ray diffraction figure of X-type zeolite at 95 DEG C;
Fig. 9:12h crystallization synthesizes the powder x-ray diffraction figure of X-type zeolite at 105 DEG C;
Figure 10:24h crystallization synthesizes the powder x-ray diffraction figure of X-type zeolite at 105 DEG C:
Figure 11:Sodium metasilicate and flyash quality than for 2.5 when crystallization synthesis X-type zeolite scanning electron microscope (SEM) photograph.
Specific embodiment
Embodiment 1.
1):Certain fly ash in electric power plant is taken, fine ash is ground to form with grinder, grain diameter is 200 mesh after grinding;
2):Product 50g after grinding is taken, is positioned in crucible, put in Muffle furnace and calcine 2h at 550 DEG C;
3):Product 30g after calcining is taken, is soaked in the 270ml hydrochloric acid solutions that concentration is 3.5mol/L, stirred at 90 DEG C Reaction 4h, then filters to it, and is washed with distilled water to pH=6.0, is dried at 105 DEG C;
4):Taking step 3) 10g after treatment dries flyash, adds 10g sodium metasilicate, 5.8g NaOH, 100ml distillations Water, is then stirred at room temperature ageing 10h, then mixture is transferred in hydrothermal reaction kettle, after good seal at 95 DEG C crystallization Reaction 8h.After the completion of reaction, room temperature is taken out and be cooled to, outwell supernatant, filter solid product, and filter cake is carried out with clear water Washing, until washing lotion pH is 8.5, with after dry at 105 DEG C, you can obtain X-type zeolite.
Synthetic zeolite scanning electron microscope (SEM) photograph is with powder x-ray diffraction figure difference as shown in Figure 6, Figure 7.Closed by crystallization at 95 DEG C Electron microscope of retouching into X-type zeolite can be seen that this octahedra zeolite be synthesized, but still suffer from circular granular form material, Zeolite purity is not high.XRD display sintetics matches with X-type zeolite characteristic diffraction peak, and angle of diffraction (2 θ) is respectively 6.479 °, 12.740 °, 15.879 °, 21.141 °, 23.819 °, 26.939 °, 36.840 °, 50.420 °, but stone in flyash English, the diffraction maximum of mullite are not wholly absent, and illustrate that the reaction does not dissolve not easily-activated quartz, mullite all, make it Participate in the middle of reaction, there is part miscellaneous peak.
Embodiment 2.
1):Certain fly ash in electric power plant is taken, fine ash is ground to form with grinder, grain diameter is 150 mesh after grinding;
2):Product 50g after grinding is taken, is positioned in crucible, put in Muffle furnace and calcine 2h at 750 DEG C;
3):Product 30g after calcining is taken, is soaked in the 300ml hydrochloric acid solutions that concentration is 4mol/L, stir anti-at 90 DEG C 5h is answered, then it is filtered, and be washed with distilled water to pH=6.0, be dried at 105 DEG C;
4):Taking step 3) 10g after treatment dries flyash, adds 15g sodium metasilicate, 5.8g NaOH, 250ml distillations Water, is then stirred at room temperature ageing 12h, then mixture is transferred in hydrothermal reaction kettle, after good seal at 95 DEG C crystallization Reaction 12h.After the completion of reaction, room temperature is taken out and be cooled to, outwell supernatant, filter solid product, and filter cake is entered with clear water Row washing, until washing lotion pH is 8.5, with after dry at 105 DEG C, you can obtain X-type zeolite.
Synthetic zeolite scanning electron microscope (SEM) photograph and powder x-ray diffraction figure are respectively as shown in Fig. 6, Fig. 8.Closed by crystallization at 95 DEG C Electron microscope of retouching into X-type zeolite can be seen that this octahedra zeolite be synthesized, but still suffer from circular granular form material, Zeolite purity is not high.XRD display sintetics matches with X-type zeolite characteristic diffraction peak, and angle of diffraction (2 θ) is respectively 6.460°、12.721°、21.141°、21.919°、26.920°、33.481°、50.439°.There is part miscellaneous peak in XRD, but with 8h reactions are compared, and relatively fully, the X zeolite RD collection of illustrative plates appearances of synthesis are more complete for 12h reactions.
Embodiment 3.
1):Certain fly ash in electric power plant is taken, fine ash is ground to form with grinder, grain diameter is 100 mesh after grinding;
2):Product 50g after grinding is taken, is positioned in crucible, put in Muffle furnace and calcine 4h at 850 DEG C;
3):Product 30g after calcining is taken, is soaked in the 300ml hydrochloric acid solutions that concentration is 4.5mol/L, stirred at 90 DEG C Reaction 5h, then filters to it, and is washed with distilled water to pH=7.0, is dried at 105 DEG C;
4):Taking step 3) 10g after treatment dries flyash, adds 15g sodium metasilicate, 5.8g NaOH, 200ml distillations Water, is then stirred at room temperature ageing 11h, then mixture is transferred in hydrothermal reaction kettle, after good seal at 105 DEG C crystallization Reaction 12h.After the completion of reaction, room temperature is taken out and be cooled to, outwell supernatant, filter solid product, and filter cake is entered with clear water Row washing, until washing lotion pH is 10.0, with after dry at 105 DEG C, you can obtain X-type zeolite.
Synthetic zeolite scanning electron microscope (SEM) photograph and powder x-ray diffraction figure are respectively as shown in Fig. 1, Fig. 9.Can by scanning electron microscope (SEM) photograph To find out, the zeolite purity of 105 DEG C of synthesis is higher, and rounded object has disappeared, and only octahedra stereochemical structure zeolite is present, and wheel Clean up clear, form is intact, uniform particle diameter.XRD display sintetics matches with X-type zeolite characteristic diffraction peak, angle of diffraction (2 θ) is respectively 6.042 °, 20.761 °, 23.381 °, 26.520 °, 31.139 °, 42.343 °, 50.057 °.
Embodiment 4.
1):Certain fly ash in electric power plant is taken, fine ash is ground to form with grinder, grain diameter is 200 mesh after grinding;
2):Product 50g after grinding is taken, is positioned in crucible, put in Muffle furnace and calcine 3h at 650 DEG C;
3):Product 30g after calcining is taken, is soaked in the 330ml hydrochloric acid solutions that concentration is 4.5mol/L, stirred at 90 DEG C Reaction 4h, then filters to it, and is washed with distilled water to pH=7.0, is dried at 105 DEG C;
4):Taking step 3) 10g after treatment dries flyash, adds 10g sodium metasilicate, 5.8g NaOH, 200ml distillations Water, is then stirred at room temperature ageing 12h, then mixture is transferred in hydrothermal reaction kettle, after good seal at 105 DEG C crystallization Reaction 24h.After the completion of reaction, room temperature is taken out and be cooled to, outwell supernatant, filter solid product, and filter cake is entered with clear water Row washing, until washing lotion pH is 9.0, with after dry at 105 DEG C, you can obtain X-type zeolite.
Synthetic zeolite scanning electron microscope (SEM) photograph is with powder x-ray diffraction figure difference as shown in Figure 1, Figure 10 shows.Can by scanning electron microscope (SEM) photograph To find out, the zeolite purity of 105 DEG C of synthesis is higher, and rounded object has disappeared, and only octahedra stereochemical structure zeolite is present, and wheel Clean up clear, form is intact, uniform particle diameter.XRD display sintetics matches with X-type zeolite characteristic diffraction peak, angle of diffraction (2 θ) is respectively 6.021 °, 12.320 °, 15.405 °, 21.439 °, 23.322 °, 26.520 °, 31.041 °, 50.020 °, at this Under the conditions of synthesize X zeolite RD collection of illustrative plates appearances it is more complete, it is preferable with what X-type zeolite standard card was matched.
Embodiment 5.
1):Certain fly ash in electric power plant is taken, fine ash is ground to form with grinder, grain diameter is 150 mesh after grinding;
2):Product 50g after grinding is taken, is positioned in crucible, put in Muffle furnace and calcine 4h at 850 DEG C;
3):Product 30g after calcining is taken, is soaked in the 300ml hydrochloric acid solutions that concentration is 4mol/L, stir anti-at 90 DEG C 4h is answered, then it is filtered, and be washed with distilled water to pH=6.0, be dried at 105 DEG C;
4):Taking step 3) 10g after treatment dries flyash, adds 25g sodium metasilicate, 5.8g NaOH, 350ml distillations Water, is then stirred at room temperature ageing 12h, then mixture is transferred in hydrothermal reaction kettle, after good seal at 105 DEG C crystallization Reaction 12h.After the completion of reaction, room temperature is taken out and be cooled to, outwell supernatant, filter solid product, and filter cake is entered with clear water Row washing, until washing lotion pH is 9.5, with after dry at 105 DEG C, you can obtain X-type zeolite.
Synthetic zeolite scanning electron microscope (SEM) photograph and powder x-ray diffraction figure are respectively as shown in Figure 11, Fig. 9.Can by scanning electron microscope (SEM) photograph Know, when sodium metasilicate and flyash quality ratio are 2.5, though the X-type zeolite of crystallization synthesis is in octahedra stereochemical structure, different topography Clearly, grain size is uniform in size, but degree of scatter is poor, major part aggregation growth, and with the presence of impurity.XRD shows Sintetics matches with X-type zeolite characteristic diffraction peak, angle of diffraction (2 θ) be respectively 6.042 °, 20.761 °, 23.381 °, 26.520°、31.139°、42.343°、50.057°。
The present invention discloses and proposes the method that simple and highly efficient flyash synthesizes X-type zeolite.Those skilled in the art Can be by using for reference present disclosure, the appropriate preparation method or treatment conditions for changing coal ash alkali heat treatment of raw materials is to be capable of achieving.It is special Not it is pointed out that all similar replacements and apparent to those skilled in the art, the Ta Mendou of change It is deemed to be included in spirit of the invention, scope and content.

Claims (8)

1. a kind of method that flyash synthesizes X-type zeolite, it is characterized in that step is as follows:
1) 100-200 mesh raw materials flyash is calcined, is obtained except the raw material after carbon;
2) by the coal-ash immersion after calcining in hydrochloric acid solution, stirring reaction, then filtering, filter cake is washed to pH=6.0- 7.0, it is then placed in oven drying;
3) to step 2) in flyash after treatment plus sodium metasilicate, NaOH and distilled water, mixed material is stirred at room temperature Ageing;It is then transferred in hydrothermal reaction kettle, seals, then hydrothermal reaction kettle is put into baking oven, is reacted at 90-105 DEG C;Instead After the completion of answering, hydrothermal reaction kettle is taken out, be cooled to room temperature, filter solid product, and filter cake is washed with distilled water, until Wash solution pH to 8.5-10, is put into oven drying after filtering, obtain X-type zeolite.
2. the method for claim 1, it is characterized in that step 1) calcining heat is 550-850 DEG C, calcination time is 2-4h.
3. the method for claim 1, it is characterized in that step 2) in, the coal-ash immersion after calcining is in 3.5-4.5mol/L Hydrochloric acid solution in, solid-to-liquid ratio uses 1:9~11 (g/ml).
4. the method for claim 1, it is characterized in that step 2) at 90 DEG C stirring reaction 4-5h.
5. the method for claim 1, it is characterized in that step 3) digestion time is 10-12h.
6. the method for claim 1, it is characterized in that step 3) material ratio is respectively:Sodium metasilicate and step 2) powder that obtains Coal ash mass ratio is 1~2.5:1, NaOH and step 2) the flyash quality ratio that obtains is fixed as 0.58:1, distill water body Product is 5.0~10 than scope with the quality of flyash and sodium silicate mixture material:1.
7. the method for claim 1, it is characterized in that step 3) reaction time is 8-24h.
8. the method for claim 1, it is characterized in that oven drying temperature is 105 DEG C.
CN201710185726.0A 2017-03-26 2017-03-26 A kind of flyash synthesizes the method for X-type zeolite Pending CN106865565A (en)

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Cited By (4)

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CN108298555A (en) * 2017-09-12 2018-07-20 柳州市柳晶科技股份有限公司 It is a kind of that the method for molecular sieve and molecular sieve obtained are manufactured using flyash
CN108722345A (en) * 2018-05-24 2018-11-02 重庆大学 A method of utilizing the zeolite and its processing high-concentration ammonia nitrogenous wastewater of flyash synthesis
CN113996142A (en) * 2021-09-08 2022-02-01 中国大唐集团科学技术研究总院有限公司华东电力试验研究院 System and method for manufacturing zeolite and capturing carbon dioxide in flue gas by using fly ash
CN115180635A (en) * 2022-08-12 2022-10-14 辽宁星空钠电电池有限公司 Method for reducing Prussian blue crystal water content by using molecular sieve

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