CN103787354B - One utilizes coal ash for manufacturing for the application of Cr (VI) ion in MCM-41 molecular sieve adsorption solution - Google Patents
One utilizes coal ash for manufacturing for the application of Cr (VI) ion in MCM-41 molecular sieve adsorption solution Download PDFInfo
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- CN103787354B CN103787354B CN201410039979.3A CN201410039979A CN103787354B CN 103787354 B CN103787354 B CN 103787354B CN 201410039979 A CN201410039979 A CN 201410039979A CN 103787354 B CN103787354 B CN 103787354B
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Abstract
The invention discloses one utilizes coal ash for manufacturing for the application of Cr (VI) ion in MCM-41 molecular sieve adsorption solution, belongs to technical field of molecular sieve preparation. The step of the present invention is: a, by former for flyash powder dry to constant weight, mix with xeraphium coal ash with HCl solution, stirring, be centrifuged, wash, dry for standby; B, step a is processed after flyash and NaOH mixed calcining, grind to form fine powder after cooling, calcined material after the grinding obtained joined in deionized water, mixing, stirring, centrifugation obtains supernatant; C, weigh template CTAB and be dissolved in deionized water, continuously stirred under water bath condition, the supernatant that dropwise obtains in dropping step b, use HNO3Regulate pH value of solution, the spawn obtained carried out crystallization, after crystallization, naturally cools to room temperature, centrifugal, washing, dry, roasting obtains MCM-41 molecular sieve. The present invention makes full use of the flyash of power plant emission as silicon and aluminum source, reduces the synthesis cost of molecular sieve, and value is high.
Description
Technical field
The present invention relates to technical field of molecular sieve preparation, more particularly, it relates to a kind of flyash utilizing power plant emission is method and the application that main silicon and aluminum source prepares MCM-41 molecular sieve.
Background technology
Mesopore molecular sieve compared with traditional micro porous molecular sieve, there is stable framing structure, duct is six side's ordered arrangement, size uniformly, there is high-specific surface area (600��1200m2��g-1), high-adsorption-capacity (> 0.7cm3��g-1), the good characteristic such as bigger aperture (2��30nm). Very big application potential is shown in fields such as selecting absorption, separation and catalysis. But comparing micro porous molecular sieve and natural zeolite material, mesostructured material generally adopts pure industrial chemicals such as silicon dioxide, sodium silicate, tetraethyl orthosilicate etc. as silicon source, cost intensive, to limit the application of molecular sieve MCM-41. The Main chemical component of flyash is A12O3��SiO2Deng, it is expected to become substituted for silicon, aluminum chemistry pure reagent carrys out the suitable feedstock of synthesizing Si-Al mesopore molecular sieve.
Through retrieval, by utilizing the flyash of power plant emission as silicon and aluminum source synthesis of molecular sieve, technical scheme to reduce molecular sieve cost is disclosed, such as Chinese Patent Application No. 200810231810.2, the applying date is on October 20th, 2008, and invention and created name is: the preparation method of a kind of SI-MCM-41 mesopore molecular sieve; Preparation method disclosed in this application case utilizes flyash for primary raw material, by using alkali Tianjin again after acid Tianjin remove impurity, obtain sodium silicate, then with sodium silicate solution for raw material, by adding template, sulfur acid for adjusting pH value, mesopore molecular sieve can be generated in sodium silicate solution, then burn template, obtain Si-MCM-41 mesopore molecular sieve.Si-MCM-41 mesopore molecular sieve prepared by this application case has mesopore and microcellular structure, there is higher specific surface area, and good absorption property, but this application case removes the metal ions such as Fe, Ca in flyash by addition sulphuric acid in the processing procedure to flyash, this kind of method is readily incorporated the sulfate ion being not easy to remove, the silicate ion produced below is produced impact, and this technical scheme still needs to further improvement.
Summary of the invention
1. invention to solve the technical problem that
It is an object of the invention to overcome the deficiency that in prior art, the preparation cost of MCM-41 molecular sieve is high, providing one utilizes coal ash for manufacturing for the application of Cr (VI) ion in MCM-41 molecular sieve adsorption solution, the present invention selects the hydrochloric acid easily removed as acid dip solution, not only can metal impurities ion in more effective removal flyash, improve the activity of powdered coal ash, simultaneously because the effumability of chloride ion, pretreated raw material will not be impacted, the MCM-41 molecular sieve performance prepared is excellent, and preparation cost is low.
2. technical scheme
For reaching above-mentioned purpose, technical scheme provided by the invention is:
The a kind of of the present invention utilizes coal ash for manufacturing for the method for MCM-41 molecular sieve, the steps include:
A, by former for flyash powder dry to constant weight, mix with xeraphium coal ash with HCl solution, stirring, be centrifuged, wash, dry for standby;
B, step a is processed after flyash and NaOH mixed calcining, grind to form fine powder after cooling, calcined material after the grinding obtained joined in deionized water, mixing, stirring, centrifugation obtains supernatant;
C, weigh template CTAB and be dissolved in deionized water, continuously stirred under water bath condition, the supernatant that dropwise obtains in dropping step b, use HNO3Regulate pH value of solution, continue to stir to obtain spawn, the spawn obtained is carried out crystallization, after crystallization, naturally cool to room temperature, centrifugal, washing, dry, roasting obtains MCM-41 molecular sieve.
Further, the mass percent concentration of HCl solution used in step a is 20%-30%, and the solid-liquid proportioning of xeraphium coal ash and HCl solution is 1:20; In centrifugally operated, centrifugal speed is 4000-6000rpm, and centrifugation time is 30-40min; Washing operation is 6��7 with deionized water wash to cleaning mixture pH.
Further, SiO contained by flyash in calcination process described in step b2Being 1:2.2 with the mass ratio of NaOH, calcining heat is 500-600 DEG C, calcination time 3-4h.
Further, after being cooled down by gained in step b, calcined material grinds to form fine powder and crosses 200-300 mesh sieve; After grinding, calcined material is 1:20 with the mass ratio of deionized water; In stirring operation, mixing time is 24 hours; In centrifugally operated, centrifugal speed is 4000-6000rpm, and centrifugation time is 20-30min.
Further, SiO in template CTAB, supernatant in step c2And H2The mol ratio of O is 0.15:1:100; Bath temperature is 35 DEG C, and the rate of addition of the supernatant obtained in step b is 1��2/s; HNO3The mass percent concentration of solution is 10%-15%, uses HNO3Regulating pH value of solution is 10��11.
Further, in step c, crystallization temperature is 100 DEG C, with the ramp of 1 DEG C/min to 550 DEG C roasting in roasting process.
The a kind of of the present invention utilizes coal ash for manufacturing for the application of MCM-41 molecular sieve, and described MCM-41 molecular sieve is for the absorption of Cr (VI) ion.
Preferably, controlling adsorption temp is 25 DEG C, Cr (VI) solion pH value is 6, in solution, Cr (VI) ion concentration is 10mg/L, adsorption time is 60min, the solid-to-liquid ratio of the dosage of MCM-41 molecular sieve and Cr (VI) solion is 1:50, Cr (VI) ion in adsorbent solution.
3. beneficial effect
Adopt technical scheme provided by the invention, compared with existing known technology, there is following remarkable result:
(1) a kind of of the present invention utilizes coal ash for manufacturing for the method for MCM-41 molecular sieve, make full use of the flyash of power plant emission as silicon and aluminum source, reduce the synthesis cost of molecular sieve, make full use of acidity and the effumability of hydrochloric acid solution, to in flyash processing procedure, the activity of powdered coal ash can not only be improved, more will not introduce new impurity;
(2) a kind of of the present invention utilizes coal ash for manufacturing for the application of MCM-41 molecular sieve, Cr (VI) ion is had good absorbability by this MCM-41 molecular sieve, 25 DEG C, pH=6 when, the clearance of Cr (VI) ion in the standard solution containing Cr (VI) ion can be reached 96.73%.
Accompanying drawing explanation
Fig. 1 is the XRD figure of the MCM-41 molecular sieve that the present invention prepares;
Fig. 2 is the N of the MCM-41 molecular sieve that the present invention prepares2Adsorption-desorption isothermal figure;
Fig. 3 is the dosage adsorption rate influence curve figure to Cr (VI) ion of the MCM-41 molecular sieve that the present invention prepares.
Detailed description of the invention
For further appreciating that present disclosure, the present invention is described in detail in conjunction with the accompanying drawings and embodiments.
Embodiment 1
In conjunction with accompanying drawing, a kind of of the present embodiment utilizes coal ash for manufacturing for the method for MCM-41 molecular sieve, and flyash used is provided by Datang Luo He thermal power plant, Huainan, and its main chemical compositions is in Table 1. Other chemical reagent mainly include cetyl trimethylammonium bromide (CTAB, analytical pure), NaOH (analytical pure), HNO3Common agents such as (analytical pure).
The chemical composition of table 1 flyash
As it can be seen from table 1 in the former powder of flyash used by the present embodiment except Si, Al composition, also have the Fe element of high level, the concrete operations of the present embodiment synthesis MCM-41 molecular sieve are:
A, weigh the former powder of 200g fly ash in electric power plant, dry at l00 DEG C to constant weight, then it is mixed with the ratio that solid-liquid proportioning (g/mL) is 1:20 with the hydrochloric acid solution that mass percent concentration is 20%, the hydrochloric acid solution that the present embodiment uses mass percent concentration to be 20% both ensure that enough HCl concentration removed foreign ion, and solid and solution can be made again to have appropriate solid-to-liquid ratio simultaneously. magnetic agitation 12h at 80 DEG C, with the centrifugal speed centrifugation 40min of 4000rpm, removing residual hydrochloric acid with deionized water wash filter cake is 7 to cleaning mixture pH, is placed in vacuum desiccator by filter cake drying standby. what deserves to be explained is, in the process of synthesis MCM-41 molecular sieve, the existence of the elements such as Fe reaction can generate precipitation in NaOH solution system, or decomposes when high temperature roast, cause that synthetic product whiteness and degree of crystallinity reduce, thus affecting the performance of synthesis of molecular sieve product. therefore, needed flyash is carried out pretreatment before synthesis MCM-41 molecular sieve. the preprocess method that the present embodiment adopts makes full use of acidity and the effumability of hydrochloric acid solution, select the hydrochloric acid easily removed as acid dip solution, not only can metal impurities ion in more effective removal flyash, clearance is more than 99.6%, remaining Si after Impurity removal, Al composition can substitute for the synthesis material of pure chemistry composition completely, the activity of powdered coal ash is greatly improved, simultaneously because the effumability of chloride ion, pretreated raw material will not be impacted, the Fe in flyash is removed compared to using sulphuric acid, the metal ions such as Ca, the clearance of the present embodiment metal impurities ion is higher, the MCM-41 molecular sieve performance prepared is more excellent.
B, weigh step a pretreated flyash 20g and 44gNaOH respectively, mix homogeneously, and in Muffle furnace, under 500 DEG C of conditions, calcine 4h, taking-up naturally cools to room temperature 30 DEG C, owing to solid particle is more thin, more big with the contact area of liquid, more it is prone to the Si in solid, Al composition dissolution extracts, calcining afterproduct is first ground to form fine powder and crosses 200 mesh sieves by the present embodiment, after grinding, calcined material mixes with deionized water by solid-liquid mass ratio (g/mL) 1:20 again, stirring 24h, centrifugation 30min under the rotating speed of 4000rpm, take supernatant, as synthesis MCM-41 molecular sieve silicon source.
C, with CTAB (cetyl trimethylammonium bromide) for template, weigh CTAB and be dissolved in deionized water, bath temperature is set to 35 DEG C, stir to solution be the light blue of homogeneous clarification. Utilize magnetic stirring apparatus in being stirred continuously process, the supernatant that dropwise dropping (1��2/s) step b obtains, SiO in template CTAB, supernatant2And H2The mol ratio of O is 0.15:1:100, is the HNO of 10% with mass percent concentration3The pH value regulating solution is 10, continues to stir aging 2h, obtains white gels. the white gels obtained is proceeded in politef reactor after 100 DEG C of crystallization 48h, naturally cool to room temperature, it is centrifugal that (the MCM-41 granule generated after crystallization cooling is very thin, except a large amount of precipitations of reunion are arranged at bottom, solution is also suspension, being centrifuged can so that solid be fully reclaimed), washing, dry, with 1 DEG C/min ramp to 550 DEG C of roastings in Muffle furnace, the present embodiment can make the relatively mild elimination of template by heating rate slowly, prevent the defect of the crystal structure caused because template removal is very fast, then constant temperature calcining 6h, namely mesoporous MCM-41 sieve sample is obtained.
The specific surface area of the MCM-41 molecular sieve that the present embodiment prepares is 596.7m2/ g, average pore size is 5.19nm, and hole wall thickness is 0.96nm, has the characteristic of typical mesostructured material. As it is shown in figure 1, as seen from Figure 1, there is a significant diffraction maximum to the XRD figure of MCM-41 molecular sieve in (100) face in sample, and this is the characteristic peak of mesostructured material, it is possible to confirmatory sample has hexagonal mesoporous arrangement architecture. It addition, can also be observed that obvious diffraction maximum in (110) face and (200) face, illustrate that the mesostructured material sample prepared by the present embodiment has good long-range order and degree of crystallinity. In Fig. 1, abscissa represents 2 �� angle of diffraction, and vertical coordinate represents diffracted intensity.
The N of the MCM-41 molecular sieve that the present embodiment prepares2Adsorption-desorption isothermal is as in figure 2 it is shown, figure it is seen that along with adsorbed gas N2With the increase of the relative pressure of carrier gas He, isothermal line occurs in that a big hysteresis loop, it was shown that this isothermal line meets Lang Gemiaoer IV type, is typical mesoporous material adsorption curve. In Fig. 2, abscissa represents relative pressure, and vertical coordinate represents adsorbance.
Cr (VI) ion is had good absorbability by the MCM-41 molecular sieve that the present embodiment prepares, wherein, controlling adsorption temp is 25 DEG C, the pH of solution is 6, in solution, Cr (VI) ion concentration is 10mg/L, adsorption time is 60min, when the solid-to-liquid ratio (g/ml) of the dosage of MCM-41 molecular sieve and Cr (VI) solion is for 1:50, MCM-41 molecular sieve is best to the absorbability of Cr (VI) ion, and the clearance of Cr (VI) ion can be reached 96.73%.
What deserves to be explained is, owing to mesostructured material is to the ion exchange mainly by its surface-Si-OH group of the adsorption of Cr (VI) ion, during pH too big (being generally higher than 8), molecular sieve can generating portion dissolve, and pH is more little, the H in solution+The Competition of ion pair adsorption potential, more than ion exchange, causes that adsorption rate is on the low side, therefore the pH value of solution removal effect when neutrality acidity somewhat on the weak side is best. And generally, industry occupies the majority containing Cr (VI) ion waste water acidity, increasing again processing cost into substantial amounts of alkali if added in advance in waste water, therefore, inventor finally determines that by test of many times the pH controlling solution is 6 the bests. In addition, inventor is drawn by theory analysis and verification experimental verification, when other conditions are identical, when in solution, Cr (VI) ion concentration is 10mg/L, it is ensured that the solid-to-liquid ratio (g/ml) of the dosage of MCM-41 molecular sieve and Cr (VI) solion is obtained in that the adsorption effect of the best for 1:50.
As it is shown on figure 3, under 25 DEG C of conditions, weigh 0.5 respectively, 1.0,1.5,2.0,2.5, MCM-41 sieve sample prepared by 3.0g the present embodiment adds in Cr (VI) solion of 100mL10mg/L, regulating pH value of solution=6, constant temperature oscillator vibration absorption 60min, after centrifugation, take supernatant, adopt Cr (VI) ion concentration after the absorption of diphenyl phosphinylidyne two hydrazine spectrophotometry. There is increase tendency along with the increase of MCM-41 dosage in the clearance of Cr (VI) ion, at the beginning owing to adsorbent amount is very few, in solution Cr (VI) ion quickly reach absorption saturated, clearance is less, increase along with MCM-41 molecular sieve dosage, adsorbed the getting more and more of Cr (VI) ion in solution, clearance increases sharply, when dosage reaches 2g, the clearance of Cr (VI) ion can reach 96.73%, being further continued for increasing dosage, clearance change slows down gradually, until substantially remaining unchanged.
Embodiment 2
The present embodiment a kind of utilizes coal ash for manufacturing for the method for MCM-41 molecular sieve and application, substantially with embodiment 1, existing preparation process is summarized as follows:
Weigh 200g coal ash of power plant, dry at l00 DEG C to constant weight, then after it being mixed for 1:20 proportioning with solid-to-liquid ratio (g/mL) with the hydrochloric acid solution that mass percent concentration is 30%, magnetic agitation 12h at 80 DEG C, centrifugal speed centrifugation 30min with 6000rpm, being 6 with deionized water wash filter cake to filtrate pH, it is standby that drying is placed in vacuum desiccator.
Weigh pre-treating fly ash 20g and 44gNaOH respectively, mix homogeneously, and in Muffle furnace 600 DEG C calcining 3h, taking-up naturally cools to room temperature, grinds to form fine powder and crosses 300 mesh sieves, and after grinding, calcined material mixes with deionized water by solid-liquid mass ratio 1:20, stirring 24h, under the rotating speed of 6000rpm, centrifugation 20min, takes supernatant, as synthesis MCM-41 molecular sieve silicon source.
With CTAB for template, according to n (CTAB): n (SiO2):n(H2The mol ratio of O)=0.15:1:100, weighs CTAB and is dissolved in deionized water, and bath temperature is set to 35 DEG C, and stirring to solution is the light blue of homogeneous clarification. Utilizing magnetic stirring apparatus in being stirred continuously process, dropwise the silicon source solution of preparation in dropping (1��2/s) step b, is the HNO of 15% by concentration3The pH value regulating solution is 10��11, continues to stir aging 2h, obtains white gels. Proceeded in politef reactor after 100 DEG C of crystallization 48h, naturally cooled to room temperature, centrifugal, washing, dry, with 1 DEG C/min ramp to 550 DEG C of roastings, then constant temperature calcining 6h in Muffle furnace, namely obtain mesostructured material sample.
Embodiment 3
The present embodiment a kind of utilizes coal ash for manufacturing for the method for MCM-41 molecular sieve and application, substantially with embodiment 1, existing preparation process is summarized as follows:
Weigh 200g coal ash of power plant, dry at l00 DEG C to constant weight, then after it being mixed for 1:20 proportioning with solid-to-liquid ratio (g/mL) with the hydrochloric acid solution that mass percent concentration is 25%, magnetic agitation 12h at 80 DEG C, centrifugal speed centrifugation 40min with 5000rpm, being 6.5 with deionized water wash filter cake to filtrate pH, it is standby that drying is placed in vacuum desiccator.
According to m (SiO2): m (NaOH)=1:2.2 proportioning, weigh pre-treating fly ash and NaOH respectively, mix homogeneously, and in Muffle furnace 500 DEG C calcining 3.5h, take out naturally cool to room temperature, grind to form fine powder and cross 300 mesh sieves, mix with deionized water by solid-liquid mass ratio 1:20, stir 24h, centrifugation 30min under 5000rpm, take supernatant, as synthesis MCM-41 silicon source.
With CTAB for template, according to n (CTAB): n (SiO2): the mol ratio of n (H2O)=0.15:1:100, weigh CTAB and be dissolved in deionized water, bath temperature is set to 35 DEG C, and stirring to solution is the light blue of homogeneous clarification. Utilizing magnetic stirring apparatus in being stirred continuously process, dropwise the silicon source solution of preparation in dropping (1��2/s) step b, is the HNO of 10% by concentration3The pH value regulating solution is 11, continues to stir aging 2h, obtains white gels. Proceeded in politef reactor after 100 DEG C of crystallization 48h, naturally cooled to room temperature, centrifugal, washing, dry, with 1 DEG C/min ramp to 550 DEG C of roastings, then constant temperature 6h in Muffle furnace, namely obtain mesostructured material sample.
A kind of described in embodiment 1��3 utilizes coal ash for manufacturing for the method for MCM-41 molecular sieve, make full use of the flyash of power plant emission as silicon and aluminum source, silicon source is extracted by pretreatment, then adopting hydro-thermal sol-gel process to prepare mesostructured material sample, comprehensive control and deep processing for flyash propose new road. Solution temperature be 25 DEG C, pH be 6, ion concentration be 10mg/L when, the maximum material removal rate of Cr (VI) ion can be reached 97.86%, being applied to sewage treatment area for MCM-41 molecular sieve and provide certain theoretical basis, using value is high.
Claims (1)
1. one kind utilizes coal ash for manufacturing for the application of Cr (VI) ion in MCM-41 molecular sieve adsorption solution, it is characterised in that: the preparation process of MCM-41 molecular sieve is:
A, drying former for flyash powder to constant weight, mix with xeraphium coal ash with the HCl solution that mass percent concentration is 20%, the solid-liquid proportioning of xeraphium coal ash and HCl solution is 1:20; Stirring, with the centrifugation 40min of 4000rpm, with deionized water wash to cleaning mixture pH be 7, dry for standby;
B, step a is processed after flyash and NaOH mixed calcining, SiO contained by flyash2Being 1:2.2 with the mass ratio of NaOH, calcining heat is 500 DEG C, calcination time 4h; Grinding to form fine powder after cooling and cross 200 mesh sieves, join in deionized water by calcined material after the grinding obtained, the mass ratio of calcined material and deionized water is 1:20; Mixing, stirring 24 hours, centrifugation obtains supernatant, and centrifugal speed is 4000rpm, and centrifugation time is 30min;
C, weigh template CTAB and be dissolved in deionized water, continuously stirred under 35 DEG C of water bath condition, the supernatant obtained in step b, SiO in template CTAB, supernatant is dropwise dripped with the speed of 1��2/s2And H2The mol ratio of O is 0.15:1:100;It is the HNO of 10% with mass percent concentration3Regulating pH value of solution is 10, continuing to stir to obtain spawn, the spawn obtained is carried out crystallization, crystallization temperature is 100 DEG C, naturally cool to room temperature after crystallization, be centrifuged, wash, dry, obtain MCM-41 molecular sieve with the ramp of 1 DEG C/min to 550 DEG C of roastings;
Controlling adsorption temp is 25 DEG C, it is 6 containing Cr (VI) solion pH value, in solution, Cr (VI) ion concentration is 10mg/L, the dosage of MCM-41 molecular sieve is 1:50 with the solid-to-liquid ratio containing Cr (VI) solion, utilizes Cr (VI) ion in the MCM-41 molecular sieve adsorption solution of preparation.
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| CN109046297A (en) * | 2018-07-26 | 2018-12-21 | 江苏开放大学（江苏城市职业学院） | A kind of preparation method and applications of modified coal ash sodium base zeolite |
| CN109704363A (en) * | 2018-12-27 | 2019-05-03 | 中国神华能源股份有限公司 | A kind of method that white clay prepares Al-MCM-41 molecular sieve |
| TWI723352B (en) * | 2019-03-13 | 2021-04-01 | 逢甲大學 | Method of incineration ash reused for synthesis of porous materials |
| CN112387299B (en) * | 2020-11-30 | 2022-02-01 | 江南大学 | Method for preparing L-furan serine by biomass chemical-enzymatic method |
| CN115818658A (en) * | 2021-09-17 | 2023-03-21 | 淮南师范学院 | Method for preparing zeolite molecular sieve by using fly ash as raw material |
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