CN108383134A - A kind of synthetic method of solid waste multi-stage porous block modenite - Google Patents
A kind of synthetic method of solid waste multi-stage porous block modenite Download PDFInfo
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- CN108383134A CN108383134A CN201810126430.6A CN201810126430A CN108383134A CN 108383134 A CN108383134 A CN 108383134A CN 201810126430 A CN201810126430 A CN 201810126430A CN 108383134 A CN108383134 A CN 108383134A
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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
- C01B39/26—Mordenite type
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- C01P2006/14—Pore volume
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2006/17—Pore diameter distribution
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Abstract
According to mass ratio it is 4~4.25 by silicon ash, metakaolin, modenite crystal seed, solid sodium hydroxide, deionized water the invention discloses a kind of synthetic method of solid waste multi-stage porous block mordenite molecular sieve:1:0.3:0.75:It 2.35~2.5 is stirred, is molded, conserving, the technical process synthesizing block mordenite molecular sieve such as hydro-thermal reaction.This method is directly silicon source using the solid waste silicon ash without any processing, Si/Al ratio is adjusted with metakaolin, by solid waste block mordenite molecular sieve；Preparation process avoids high-temperature roasting and decomposes high energy consumption and environmental pollution caused by template it is not necessary that template is added；Meanwhile the block molecular sieve synthesized overcomes many puzzlements of filtering in powder particle application process, separation, and the feature with multistage pore canal.Building-up process simple process and low cost it is honest and clean, it can be achieved that Industrial Solid Waste and natural minerals high value added utilization.
Description
Technical field
The invention belongs to the preparations of zeolite molecular sieve and its solid waste resource recovery to utilize field, be related to the conjunction of molecular sieve
At, and in particular to a kind of synthetic method of solid waste silicon ash green resource multi-stage porous block modenite.
Background technology
Silicon ash is the byproduct during the alloy smeltings such as metallic silicon or ferrosilicon, usual white or grey, specific surface area
Greatly, there is high activity[1-2].Contain a large amount of active silica in silicon ash, carrying out recycling not only to it can be reduced
Environmental pollution is improved the ecological environment, moreover it is possible to be turned waste into wealth, is one of the important channel of silicon industrial sustainable development.
Currently, silicon ash is mainly used in concrete admixture[3], cement mixture[4], refractory material[5]Equal fields.It utilizes
Silicon ash synthesis of molecular sieve has had related report.It is mainly using the molecular sieve of Template synthesis powder.Chen Xiuhua[6]Et al.
By silicon ash, template (4-propyl bromide, tetrapropylammonium hydroxide), ammonium hydroxide, sodium chloride with molar ratio for 1:0.1:0.039~
0.052:0~2 mixing, ultrasonic vibration 2.5h, for 24 hours, reaction product is washed, filters, 60 DEG C of dry 12h for 160 DEG C of hydrothermal crystallizings
Obtain including the micropore ZSM-5 molecular sieve of organic formwork agent.Chen Xiuhua[7]Et al. by wollastonite powder, sodium metasilicate, template (tetrapropyl
Ammonium bromide) and alkali source (ammonium chloride or ammonium fluoride) mass ratio be 1:1.315:0.12~0.24:0.43 ground and mixed, 130~
12~48h of crystallization at 160 DEG C, reaction product is ground, dissolving, filter, drying obtains micropore ZSM-5 molecular sieve.Marvin's
Meeting[8]Et al. reported using SILICA FUME prepare SiO2Molecular sieve.Heat treatment 5h is carried out to SILICA FUME at 500 DEG C first, to remove
Carbon and other volatile impurities, then carry out acidleach processing with hydrochloric acid, remove acid soluble impurities, by acidleach treated wollastonite powder with
NaOH, template (cetyl trimethylammonium bromide, hexadecyltrimethylammonium chloride, polyethylene glycol, F127, organic additive
For ethyl alcohol or triethanol ammonium) and H2O in molar ratio 1:0.2~0.4:0.1~0.3:150~200 mixing, at 90 DEG C~120 DEG C
Under the conditions of, 12~48h is reacted, then by washing, filtering, drying, obtains Organic-inorganic composite intermediate product；By this is organic-
Inorganic compounding intermediate product is with water according to mass ratio 1:It is stirred after 30~50 mixing, and carries out hydro-thermal process, the solid that will be obtained
The mesoporous SiO of powder is made in matter detergent, filtering and drying, 400 DEG C of -700 DEG C of roasting 5-8h, removed template method2Molecular sieve.
Wang Yuanhui[9]Etc. having reported a kind of synthetic method of SSZ-13 zeolite molecular sieves.By SILICA FUME, silicon source, (18 water closes
Aluminum sulfate), NaOH, template (N, N, N- trimethyl adamantane ammonium hydroxide, copper-amine complex), water according to the ratio 5~100:1:
10~50:2~15:200~20:60 are mixed, and 140 DEG C~165 DEG C 48~54h of hydro-thermal reaction are filtered, are dried to obtain SSZ-
13 zeolite molecular sieve original powders；By 550 DEG C of roasting 5h of the original powder, the SSZ-13 zeolite molecular sieves of removed template method are obtained.Chen Jie
Chongqing[10]Et al. reported it is a kind of using SILICA FUME synthesize 4A zeolite molecular sieves method, by SILICA FUME, sodium aluminate, sodium hydroxide
Meet molar ratio Si/Al (1~1.5 with the addition of water:1), (1~2 Na/Si:1),H2O/Si (50~100:1) it mixes, magnetic
Under power stirring, 80~100 DEG C of 6~12h of reaction, room temperature is aged 4~12h, vacuum filtration washing, and 4A zeolites are made in 105 DEG C of drying
Molecular sieve.
It is above-mentioned that there are two big features using silicon ash synthesis of molecular sieve：One, in the building-up process of molecular sieve, it is necessary to be added
Organic formwork agent；Secondly, the molecular sieve that synthesizes be powder granule.
Modenite is a kind of natural zeolite, is had a wide range of applications in fields such as catalysis, ion exchange, absorption[11-13]。
1948, Barrer etc. [14] was using sodium carbonate as mineralizer, by silicic acid gel and sodium aluminate aqueous solution hydro-thermal at 265-295 DEG C
Crystallization, it is artificial synthesized for the first time go out modenite.Up to the present, the synthesis of modenite is mainly using Ludox or sodium metasilicate as silicon
Source, sodium metaaluminate or sodium aluminate are silicon source[15-17]。
In conclusion applicant is not had found by a large amount of domestic patent of system reviews and documents and materials with solid
Useless silicon ash is silicon source, and Si/Al ratio is adjusted with metakaolin, the correlation of solid waste synthesizing flokite is reported, more without block silk
The related report of light boiling synthesis.
It is the relevant references that inventor provides below：
[1] Khan M.I., Siddique R., Utilization of silica fume in concrete:
Review of durability properties, Resources Conservation＆Recycling, 2011,57 (4):
30-35。
[2] Sun Ning, Li Junhan, Yang Shaoli, Jiang Peng, Zhu Hongjia, the performance and purposes of ferroalloy smelting by-product SILICA FUME,
Henan chemical industry, 2017,34 (4):7-10.
[3] Memon F.A., Nuruddin M.F., Shafiq N., Effect of silica fume on the
fresh and hardened properties of fly ash-based self-compacting geopolymer
Concrete, International Journal of Minerals, Metallurgy and Materials, 2013,20
(2):205-213。
[4] He Zhiyong, Peng little Yan, Wang Suzhen, Zeng Zhenyu, the influence of Microsilica on Flowability of Ultra-Low Cement Castable, silicon
Hydrochlorate is notified to, 2005,24 (6):53-55.
[5] Li Z.Yu, Q., Chen X., Liu H., Zhang J., Zhang J., Yang Y., Wei J., The
role of MgO in the thermal behavior of MgO–silica fume pastes,Journal of
Thermal Analysis＆Calorimetry, 2017,127 (3):1897-1909.
[6] Chen Xiuhua, Lei Zhengtao, red legend is outstanding, Marvin's meeting, a method of ZSM-5 molecular sieve being synthesized using SILICA FUME,
CN105984885A, 2016.
[7] Chen Xiuhua, Lei Zhengtao, red legend are outstanding, a method of using SILICA FUME synthesis in solid state ZSM-5 molecular sieve,
CN106006670A, 2016.
[8] Marvin's meeting, red legend is outstanding, and Wei Kuixian, Li Mingming, Zhouyang, Yu Jie, Xie Keqiang, Wu Jijun, Qin Bo, Lu Kingdom is strong, and one
The preparation method of kind SiO 2 molecular sieve, CN103539147A, 2014.
[9] Wang Yuanhui, Chen Jieyu, department's will dawn, Lei Xinrong, a kind of side synthesizing SSZ-13 zeolite molecular sieves using SILICA FUME
Method, CN106587097A, 2017.
[10] Chen Jieyu, Lei Xinrong, Wang Yuanhui, a method of 4A zeolite molecular sieves being synthesized using SILICA FUME,
CN106335908A, 2017.
[11] Yang Rui, Mo Jinhan, Zhang Yinping, TiO2The formaldehyde degradation by photocatalytic oxidation process characteristic research of/modenite, Engineering Thermophysics
Journal, 2005,26 (3):474-476.
[12] Wang Guanghuo, Mo Huiming, Zhu Zuxiang, research of the natural zeolite as ion exchange fertilizer, Zhejiang Agricultural Univ
Journal, 1990,16 (3):225-228.
[13] Zhang Dongna, Song Yonghui, bow love monarch, Yuan Peng, Peng Jianfeng adsorb grinding for ammonia nitrogen in high density using modenite
Study carefully, safety and environment journal, 2006,6 (5):17-20.
[14] Barrer R.M., Synthesize and reactions of mordenite, Journal of
Chemical Soceity, 1948,24 (6):2158-2163.
[15] Wang Jian, Jin Xingmei, influence of the synthesis condition to modenite crystallinity, petrochemical industry, 2004,33:27-
29。
[16] Zhang Yanfeng, Xu Zhongqiang, Chen Qingling, the preparation and representation of microcrystal mordenites film, catalysis journal, 2002,
23(2):145-149。
[17] it is strict just, Lin Ruisen, chrysanthemum ground English one, the positive man of virtue and ability of loose measure, the preparation of mordenite membrane and its influence factor, Zhejiang
River college journal (Edition), 2005,32 (4):423-427.
Invention content
The object of the present invention is to provide one kind to be guided with crystal seed, by solid waste silicon ash multi-stage porous block modenite molecule
The method of sieve.
In order to realize that above-mentioned task, the present invention take following technical solution：
A kind of synthetic method of solid waste multi-stage porous block mordenite molecular sieve, which is characterized in that by silicon ash, higher ridge
Soil, modenite crystal seed, sodium hydroxide aqueous solution be put into agitating device carry out mix formed slurry, by mold molding,
Maintenance, demoulding, obtains block；Then block is placed in crystallization in reaction kettle and obtains multi-stage porous block mordenite molecular sieve；Its
In：Silicon ash, metakaolin, modenite crystal seed, solid sodium hydroxide, deionized water mass ratio be 4~4.25:1:0.3:
0.75:2.35~2.5.
Specifically implement according to the following steps：
(1) silicon ash is weighed by formula ratio, be placed in blender；
(2) metakaolin is weighed by formula ratio, be placed in blender；
(3) modenite crystal seed is weighed by formula ratio, be placed in blender, silicon ash, metakaolin and modenite is brilliant
Kind three forms mixture after being mixed evenly；
(4) solid sodium hydroxide is weighed by formula ratio；
(5) deionized water is weighed by formula ratio, solid sodium hydroxide is dissolved in deionized water；
(6) aqueous solution of sodium hydroxide is placed in blender, is stirred evenly with the mixture in step (3), formed equal
Even slurry；
(7) slurry is contained into die for molding, mold is sealed with plastic film hermetic bag, is placed in 50 DEG C of maintenances in insulating box
For 24 hours, it then takes out, demoulds, obtain block；
(8) block is placed in reaction kettle, be added 75mL deionized waters, seal kettle, in 180 DEG C of hydro-thermal reactions for 24 hours~
48h then takes out, and washs, dry, obtains multi-stage porous block mordenite molecular sieve.
The synthetic method of the solid waste multi-stage porous block mordenite molecular sieve of the present invention, creatively proposes direct utilization
Solid waste silicon ash without any processing is silicon source, and Si/Al ratio, crystal seed guiding, by solid waste multi-stage porous block are adjusted with metakaolin
Organic formwork agent need not be added in building-up process in mordenite molecular sieve, avoid caused by high-temperature roasting decomposes template
High energy consumption and environmental pollution；Meanwhile the block molecular sieve synthesized overcome in powder particle application process be separated by filtration it is all
More puzzlements.Building-up process simple process and low cost it is honest and clean, it can be achieved that Industrial Solid Waste and natural minerals high value added utilization, application
It has a extensive future.
Description of the drawings
Fig. 1 is the photo in kind of multi-stage porous block mordenite molecular sieve；
Fig. 2 is scanning electron microscope (SEM) photo of multi-stage porous block mordenite molecular sieve；
Fig. 3 is X-ray diffraction (XRD) collection of illustrative plates of block mordenite molecular sieve；
Below in conjunction with drawings and examples, the present invention is described in further detail.
Specific implementation mode
It should be noted that embodiment below, just to preferably annotate the present invention, the present invention is not restricted to these implements
Example.
The present embodiment provides a kind of synthetic method of solid waste multi-stage porous block mordenite molecular sieve, raw material using silicon ash,
Metakaolin, modenite crystal seed, solid sodium hydroxide and deionized water, also, silicon ash, metakaolin, modenite are brilliant
The mass ratio of kind, sodium hydroxide and deionized water is 4~4.25:1:0.3:0.75:2.35~2.5.
(1) silicon ash is purchased from Inner Mongol Huhehaote City Fujian new energy materials Co., Ltd.
The main oxides composition (mass percent) of silicon ash：SiO2(86.25%), CaO (0.68%), Al2O3
(0.73%), Na2O (0.85%), MgO (1.31%), K2O (2.08%), Fe2O3(7.08%), LOI (1.02%).
(2) metakaolin is purchased from Chen Yinaicai abrasive materials Co., Ltd of Gongyi City.
The main oxides composition (mass percent) of metakaolin：SiO2(55.06%), CaO (0.17%), Al2O3
(44.12%), TiO2(0.24%), MgO (0.06%), K2O (0.55%), Na2O (0.06%), Fe2O3(0.76%), LOI
(0.62%).
(3) modenite crystal seed, silica alumina ratio 50 are purchased from Yangzhou and Co., Ltd of petrochemical industry research institute.
(4) solid sodium hydroxide is purchased from Sinopharm Chemical Reagent Co., Ltd., analytical reagents, molecular weight 40g/
mol。
(5) deionized water, laboratory self-control.
(6) specifically implement according to the following steps：
1) silicon ash is weighed by formula ratio, be placed in blender；
2) metakaolin is weighed by formula ratio, be placed in blender；
3) modenite crystal seed is weighed by formula ratio, be placed in blender, by silicon ash, metakaolin and modenite crystal seed
Three forms mixture after being mixed evenly；
4) solid sodium hydroxide is weighed by formula ratio；
5) deionized water is weighed by formula ratio, solid sodium hydroxide is dissolved in deionized water；
6) aqueous solution of sodium hydroxide is placed in blender, is stirred evenly with the mixture in step 3), formed uniform
Slurry；
7) slurry is contained into die for molding, mold is sealed with plastic film hermetic bag, is placed in 50 DEG C of maintenances in insulating box
For 24 hours, it then takes out, demoulds, obtain block；
8) block is placed in reaction kettle, be added 75mL deionized waters, seal kettle, in 180 DEG C of hydro-thermal reactions for 24 hours~48h,
It then takes out, washs, it is dry, obtain multi-stage porous block mordenite molecular sieve.
It is the specific embodiment that inventor provides below.
Embodiment 1：
Precise silicon ash, metakaolin, modenite crystal seed, sodium hydroxide, deionized water, mass ratio 4:1:
0.3:0.75:2.35.Silicon ash, metakaolin and modenite crystal seed are placed in blender and stir into mixture；By solid hydrogen
Sodium oxide molybdena dissolves in deionized water, then, sodium hydrate aqueous solution is poured into the blender for fill mixture and is stirred again,
Form uniformly mixed slurry；Slurry is fitted into six steel dies of 2cm × 2cm × 2cm, the jolt ramming on glue sand plain bumper；
Mold is sealed with plastic film hermetic bag, is placed in 50 DEG C of maintenances in insulating box and for 24 hours, is then taken out demoulding, obtain block test specimen, will
Block test specimen is put into reaction kettle, and 75mL deionized waters are added, and seals kettle；180 DEG C of hydro-thermal reactions for 24 hours, are taken out washing, drying, are obtained
To multi-stage porous block mordenite molecular sieve.A figures in Fig. 1 show the obtained multi-stage porous block modenite of the present embodiment
The photo in kind of molecular sieve；Fig. 2 shows scanning electron microscope (SEM) photo of multi-stage porous block mordenite molecular sieve, from Fig. 2
As can be seen that multi-stage porous block mordenite molecular sieve is made of nanoprisms crystal；Fig. 3 shows block modenite
X-ray diffraction (XRD) collection of illustrative plates of molecular sieve, from XRD spectrum as it can be seen that the block of synthesis belongs to pure mordenite molecular sieve crystalline substance
Object constructional features
Table 1 gives the pore-size distribution of multi-stage porous block mordenite molecular sieve, as seen from Table 1, multi-stage porous block mercerising
There is zeolite molecular sieve aperture (＜ 2nm), mesoporous (2~50nm), macropore (＞ 50nm) structure, wherein aperture pore volume to account for total hole
The 7.28% of volume, mesoporous pore volume account for the 60.48% of total pore volume, and macropore pore volume accounts for the 32.24% of total pore volume, shows
The block mordenite molecular sieve of synthesis has hierarchical porous structure.
Table 1：The pore-size distribution of multi-stage porous block mordenite molecular sieve
Embodiment 2：
Precise silicon ash, metakaolin, modenite crystal seed, sodium hydroxide, deionized water, mass ratio 4:1:
0.3:0.75:2.35.Silicon ash, metakaolin and modenite crystal seed are placed in blender and stir into mixture；By solid hydrogen
Sodium oxide molybdena dissolves in deionized water, then, sodium hydrate aqueous solution is poured into the blender for fill mixture and is stirred again,
Form uniformly mixed slurry；Slurry is fitted into six steel dies of 2cm × 2cm × 2cm, the jolt ramming on glue sand plain bumper；
Mold is sealed with plastic film hermetic bag, is placed in 50 DEG C of maintenances in insulating box and for 24 hours, is then taken out demoulding, obtain block test specimen, will
Block test specimen is put into reaction kettle, and 75mL deionized waters are added, and seals kettle；180 DEG C of hydro-thermal reaction 48h take out washing, drying, obtain
To multi-stage porous block mordenite molecular sieve.B figures in Fig. 1 show the obtained multi-stage porous block modenite of the present embodiment
The photo in kind of molecular sieve.
Embodiment 3：
Precise silicon ash, metakaolin, modenite crystal seed, sodium hydroxide, deionized water, mass ratio 4.25:
1:0.3:0.75:2.5.Silicon ash, metakaolin and modenite crystal seed are placed in blender and stir into mixture；By solid hydrogen
Sodium oxide molybdena dissolves in deionized water, then, sodium hydrate aqueous solution is poured into the blender for fill mixture and is stirred again,
Form uniformly mixed slurry；Slurry is fitted into six steel dies of 2cm × 2cm × 2cm, the jolt ramming on glue sand plain bumper；
Mold is sealed with plastic film hermetic bag, is placed in 50 DEG C of maintenances in insulating box and for 24 hours, is then taken out demoulding, obtain block test specimen, will
Block test specimen is put into reaction kettle, and 75mL deionized waters are added, and seals kettle；180 DEG C of hydro-thermal reactions for 24 hours, are taken out washing, drying, are obtained
To multi-stage porous block mordenite molecular sieve.C figures in Fig. 1 show the obtained multi-stage porous block modenite of the present embodiment
The photo in kind of molecular sieve.
Claims (5)
1. a kind of synthetic method of solid waste multi-stage porous block mordenite molecular sieve, which is characterized in that by silicon ash, metakaolin,
Modenite crystal seed, sodium hydroxide aqueous solution be put into agitating device carry out mix formed slurry, by mold molding, support
Shield, demoulding, obtains block；Then block is placed in crystallization in reaction kettle and obtains multi-stage porous block mordenite molecular sieve；Wherein：
Silicon ash, metakaolin, modenite crystal seed, solid sodium hydroxide, deionized water mass ratio be 4~4.25:1:0.3:0.75:
2.35~2.5.
2. the method as described in claim 1, which is characterized in that specifically implement according to the following steps：
(1) silicon ash is weighed by formula ratio, be placed in blender；
(2) metakaolin is weighed by formula ratio, be placed in blender；
(3) modenite crystal seed is weighed by formula ratio, be placed in blender, by silicon ash, metakaolin and modenite crystal seed three
Person forms mixture after being mixed evenly；
(4) solid sodium hydroxide is weighed by formula ratio；
(5) deionized water is weighed by formula ratio, solid sodium hydroxide is dissolved in deionized water；
(6) aqueous solution of sodium hydroxide is placed in blender, is stirred evenly with the mixture in step (3), formed uniform
Slurry；
(7) slurry to be contained into die for molding, mold is sealed with plastic film hermetic bag, is placed in insulating box and is conserved for 24 hours for 50 DEG C,
It then takes out, demoulds, obtain block；
(8) block is placed in reaction kettle, be added 75mL deionized waters, seal kettle, in 180 DEG C of hydro-thermal reactions for 24 hours~48h, so
After take out, wash, it is dry, obtain multi-stage porous block mordenite molecular sieve.
3. method as claimed in claim 1 or 2, which is characterized in that the main oxides mass percent of the silicon ash forms
For：SiO2：86.25%, CaO：0.68%, Al2O3：0.73%, Na2O：0.85%, MgO：1.31%, K2O：2.08%,
Fe2O3：7.08%, LOI：1.02%.
4. method as claimed in claim 1 or 2, which is characterized in that the main oxides mass percent of the metakaolin
Group becomes：SiO2：55.06%, CaO：0.17%, Al2O3：44.12%, TiO2：0.24%, MgO：0.06%, K2O：0.55%,
Na2O：0.06%, Fe2O3：0.76%, LOI：0.62%.
5. multi-stage porous block mordenite molecular sieve made from one of claim 1-4 the methods.
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Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040187740A1 (en) * | 2003-03-27 | 2004-09-30 | Research Incubator, Ltd. | Cementitious composition |
| CN100436320C (en) * | 2006-05-08 | 2008-11-26 | 浙江大学 | Method for synthesizing high-silicon mordenite in the absence of amine |
| JP5132508B2 (en) * | 2008-09-29 | 2013-01-30 | 電気化学工業株式会社 | Cement admixture and cement composition |
| CN104909384B (en) * | 2015-05-27 | 2017-01-25 | 中国科学院广州地球化学研究所 | Mordenite having diatomite morphology and multi-level pore channel structure, and preparation method thereof |
| CN106185976A (en) * | 2016-07-22 | 2016-12-07 | 太原理工大学 | A kind of multi-stage porous mordenite molecular sieve and preparation method thereof |
| CN107311193B (en) * | 2017-08-16 | 2019-11-12 | 西南科技大学 | A kind of preparation method of pollucite tiny balloon |
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