CN105731486B - The method that spherical analcime mesoporous material is prepared using low-quality attapulgite clay mine tailing - Google Patents
The method that spherical analcime mesoporous material is prepared using low-quality attapulgite clay mine tailing Download PDFInfo
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Abstract
The invention discloses the method for preparing spherical analcime mesoporous material using low-quality attapulgite clay mine tailing, it is characterized in that the attapulgite clay mine tailing that grade is low, complicated component, absorption property are poor is changed into the homogeneous micron-size spherical mesoporous adsorption material controllable, absorption property is excellent of pore-size distribution by a step hydro-thermal reaction.The present invention is not on the premise of organic surface active agent class pore former is introduced, the crystal structure of attapulgite and state of aggregation are changed by a step hydro-thermal reaction, simultaneously by the dissolving crystallized restructuring of associated mineral, obtain the mesoporous analcime material with micron-size spherical form, product aperture narrowly distributing, technique is simple, properties of product are stable, pore-size distribution is controllable, absorption property is excellent, and the numerous areas such as the enrichments of precious metal ion such as efficient absorption removal and rubidium, the caesium of antibiotic, mycotoxin, dyestuff and heavy metal are widely used in as adsorbent.
Description
Technical field
The present invention relates to a kind of method that spherical analcime mesoporous material is prepared using low-quality attapulgite clay mine tailing, category
In nonmetallic ore deep processing and mesoporous nano field of material synthesis technology.
Background technology
China, which possesses, accounts for world's gross reserves attapulgite clay resource of more than half, but because the attapulgite in China sticks
Tu Kuang is resulted from Middle Cenozoic continental basins mostly, and main preservation is in Tertiary Stratigraphy, based on the gyittja origin cause of formation.It is recessed
Convex rod stone is in forming process because the change of geological conditions, often symbiosis simultaneously go out many other mineral, the presence of which
The crystal development degree of attapulgite can be had an impact, and finally influence the chemical composition of attapulgite, rod crystal structure and make
Use performance.Therefore, attapulgite content is between 10%~80% in China's attapulgite clay ore deposit, and wherein content is less than 40%
Low-grade ore it is in the majority, cause added value of product relatively low, resource utilization is not high.
In recent years, attapulgite research receives the extensive concern of domestic scholars, and researcher is from different angles to resource
Research has been carried out in distribution, physical and chemical performance, surface modification, Organic-inorganic composite and mineral composition etc., but current research is more
Surface modification treatment and function and service etc. are concentrated on, with regard to how to change attapulgite rod crystal structure and then prepare new and effective
The key technology research and development of function nano material are related to few.Therefore, prior art can not still utilize low-grade attapulgite clay
Miscellaneous ore deposit develops high-end product, and most low-grade ores are caused the serious waste of resource, seriously constrained production by as tailings glass
The development of industry.
Analcime is a kind of microporous crystalline silico aluminate with three-dimensional screen work, has larger specific surface area and higher
The heavy metal ion exchange capacity such as lead, copper.Therefore, analcime can be used for extraction heavy metal ion, sewage disposal, heavy metal polluted soil
The field such as the repairing and treating of earth and fine chemistry industry.But the natural reserves of analcime are very low, only originate in the U.S., Japan and China etc.
A few countries, therefore most analcime production needs are artificial synthesized at present.Ghobarkar etc.（Materials Science
And Engineering, 1999, B60：163-167）The analcime crystal of 50nm~100 μm is prepared with hydro-thermal method；In
The A of state patent CN 103572362 are disclosed using sodium metasilicate, sodium hydroxide, silica flour, aluminium powder as raw material, are synthesized using hydro-thermal method
A kind of cubic system analcime monocrystal, size are about 100μM, but direct synthesis technique is because using chemical reagent as raw material, synthesizing cost
It is higher.The A of patent CN 103046111 disclose one kind using flyash as raw material, and a kind of nanoscale side has been synthesized using hydro-thermal method
Zeolite, reduce synthesis cost；Atta etc.（Applied Clay Science, 2012,61：8–13）With kaolin and rice husk
Ash is raw material, the spherical analcime of multiaspect using hydro-thermal one pot process；Ma etc.（Microporous and Mesoporous
Materials, 2015,201：134–140）Using quartz-orthoclase as raw material, square boiling has equally been synthesized using hydro-thermal alkaline etching method
Stone.Attapulgite ideal structure formula is（Al2Mg2）Si8O20（OH）2（OH2）4·4H2O, natural silicon source and silicon source can be used as to synthesize
Analcime.Therefore, analcime material is directly synthesized using natural attapulgite clay mineral resource, can not only obtains high property
The analcime material of energy, low cost, and open up new way for low-quality attapulgite clay resource high-value-use.
Also there is research to confirm that high-purity attapulgite can change to analcime at present.Zhang Pingping etc.（Material science and work
Journey journal, 28（4）：501-504）Using the attapulgite of purification as raw material, direct alkali solution technique, template agent method and molten is respectively adopted
Glue-hydro-thermal method makes attapulgite change to analcime.The chemical composition of used purification attapulgite is SiO2, 26.37%；
Al2O3, 10.32%；Fe2O3, 4.36%；MgO, 17.16%；CaO, 18.14%.Its content of MgO reaches 17.16%, is typical height
Grade attapulgite clay.From the aspect of raw material, the raw materials used high-purity attapulgite higher for cost（Attapulgite content
81%）.Seen in process aspect, preprocessing process complexity is, it is necessary to consume substantial amounts of acid and water, and need substantial amounts of alkali or template
Agent, reaction temperature are higher.From the aspect of product structure analysis, direct alkali fusion obtains in product it is observed that analcime feature
Peak, quartz content reduce, but attapulgite peak weakens but do not disappeared, or even the peak does not all disappear after 200 DEG C of reactions, illustrates bumps
The conversion of rod stone is incomplete, and obtained product is analcime, quartz and attapulgite mixture.
Zhang Pingping etc.（Chinese Journal of Inorganic Chemistry, 2009,25（09）：1545-1550）Alkaline etching be also studied to attapulgite
The influence of structure, it is found that attapulgite structure develops, there is analcime generation in the product, but analcime is only accessory substance,
And attapulgite does not convert completely, what is obtained is attapulgite and analcime mixture.Therefore, by low-grade attapulgite
Clay is completely transformed into analcime by simple single step reaction, prepares high-purity analcime, will be to low-grade attapulgite
The high-value-use of clay is significant, but there is no relevant report at present.
The content of the invention
The purpose of the present invention is：One kind is provided and prepares spherical analcime mesoporous material using low-quality attapulgite clay mine tailing
Method, a small amount of inorganic salts only need to be introduced in hydrothermal reaction process, so that it may induce in attapulgite clay each component to recombinate shape
Glomerate mesoporous analcime, miscellaneous ore deposit and attapulgite are changed into jointly in course of reaction preferable absorption property and higher steady
Qualitatively mesoporous material, the target that high-performance adsorbent is prepared using attapulgite clay is not only realized, and be low-grade recessed
The higher value application of convex rod stone clay opens up new way.
The present invention technical solution be：Powder is made in the attapulgite clay mine tailing of low-quality, by solid-to-liquid ratio 1:60~
1:6 are distributed in the modifier aqueous solution containing 1 ~ 20% mass fraction, then are aged 1-12h after being ultrasonically treated 65 min, are transferred to
In the hydro-thermal reaction tank of sealing, in 100 ~ 199 °C of MPa of pressure 1.5 ~ 6, temperature h of condition hydro-thermal reaction 4 ~ 100, product is divided
From, dry, crush, obtain the mesoporous analcime material of the homogeneous microspheroidal of pore-size distribution.
Wherein, described low-quality attapulgite clay mine tailing is low-grade ore and powder, and its chemical composition range is：
Al2O3, 10.5% ~ 26%；MgO, 2.5% ~ 9%；SiO2, 45% ~ 80%.
Wherein, described modifying agent is sodium thiosulfate, sodium polysulfide, sodium sulfite, sodium hydrogensulfite, sodium sulphate, sulphur
Change sodium, sodium carbonate, sodium acid carbonate, potassium sulfide, potassium thiosulfate, potassium sulfite, potassium bisulfite, potassium sulfate, potassium carbonate, carbonic acid
At least one of hydrogen potassium, sodium metaaluminate, sodium hypochlorite, aluminium hydroxide.
Wherein, described modifying agent accounts for attapulgite clay mine tailing mass percent as 1 ~ 20%；Attapulgite clay ore deposit
The solid-to-liquid ratio of powder and reaction solution is 1:60~1:6.
Wherein, described reaction pressure is 1.5 ~ 6 MPa, and reaction temperature is 100 ~ 199 °C, and the reaction time is 4 ~ 100 h.
Wherein, described reactant mixture is aged 1-12h after being ultrasonically treated 65 min.
Compared with the conventional method, the present invention has advantages below：
1st, the raw material used is China's rich reserves but is difficult to the low-quality attapulgite clay raw ore of high-value-use, is not required to
Complicated acid treatment program is wanted, attapulgite and association in low-quality attapulgite clay are only achieved that by a step hydro-thermal reaction
The restructuring of ore deposit crystal structure forms the spherical analcime with meso-hole structure；
2nd, the preparation method technique is simple, and process is easily controllable, and product quality is stable, obtained nanoporous adsorbent pores
Footpath distribution is homogeneous, stable and aperture is controllable.
3rd, the present invention has synthesized Jie that reserves are rare in nature using the low-quality attapulgite clay resource of rich reserves
Hole analcime material, and applied to the adsorbing separation of the material such as heavy metal, dyestuff, it is a kind of to meet the green of sustainable development requirement
Color new technology, while open up new way for the higher value application of attapulgite clay.
Brief description of the drawings
Fig. 1 is the XRD spectrum of attapulgite clay and spherical analcime；
Fig. 2 is attapulgite clay and spherical analcime stereoscan photograph；
Fig. 3 is attapulgite clay and spherical analcime pore size distribution curve；
Fig. 4 is the absorption property curve of attapulgite clay and spherical analcime to methylene blue；
Fig. 5 is the absorption property curve of attapulgite clay and spherical analcime to tetracycline；
Fig. 6 is the absorption property curve of attapulgite clay and spherical analcime to aureomycin.
Embodiment
With reference to embodiment to the present invention technical solution be described further, these embodiments it is not intended that
It is the limitation to technical scheme.
Embodiment 1：By 100 g attapulgite clay（Al2O3, 10.5%；MgO, 2.5%；SiO2, 80%）It is scattered in 600
In the aqueous solution of mL vulcanized sodium containing 1g, stirring and dissolving, 65min is ultrasonically treated, is aged 12h, be transferred to the hydrothermal reaction kettle of 5 L sealings
In, in 199 °C of MPa of pressure 6, temperature h of conditioned response 100, product obtains spherical side after centrifuging, dry, crush
Zeolite mesoporous material.
Embodiment 2：By 50 g attapulgite clay（Al2O3, 16%；MgO, 9%；SiO2, 70%）3000 mL are scattered in contain
In the aqueous solution of 7.5g sodium carbonate and 2.5 g potassium sulfides, stirring and dissolving, 65 min are ultrasonically treated, are aged 1h, be transferred to 5 L sealings
Hydrothermal reaction kettle in, in 100 °C of MPa of pressure 1.5, temperature h of conditioned response 100, product is by centrifuging, drying, powder
After broken, spherical analcime mesoporous material is obtained.
Embodiment 3：By 100 g attapulgite clay（Al2O3, 26%；MgO, 9%；SiO2, 55%）3000 mL are scattered in contain
In the aqueous solution of 8g sodium sulfites and 7 g sodium metaaluminates, stirring and dissolving, 65 min are ultrasonically treated, are aged 6h, be transferred to 5 L sealings
Hydrothermal reaction kettle in, in 180 °C of MPa of pressure 3, temperature h of conditioned response 20, product is by centrifuging, drying, crushing
Afterwards, spherical analcime mesoporous material is obtained.
Embodiment 4：By 300 g attapulgite clay（Al2O3, 14%；MgO, 6.5%；SiO2, 68%）It is scattered in 3000 mL
In the aqueous solution containing 10 g sodium hydrogensulfites and 5 g vulcanized sodium, stirring and dissolving, 65 min are ultrasonically treated, are aged 8h, are transferred to 5 L
In the hydrothermal reaction kettle of sealing, in 160 °C of MPa of pressure 6, temperature h of conditioned response 48, product by centrifuging, drying,
After crushing, spherical analcime mesoporous material is obtained.
Embodiment 5：By 200 g attapulgite clay（Al2O3, 14%；MgO, 6.5%；SiO2；75%）It is scattered in 4000 mL
In the aqueous solution of sodium acid carbonate containing 10g and 10 g potassium sulfites, stirring and dissolving, 65 min are ultrasonically treated, are aged 12h, are transferred to 5 L
In the hydrothermal reaction kettle of sealing, in 180 °C of MPa of pressure 4, temperature h of conditioned response 24, product by centrifuging, drying,
After crushing, spherical analcime mesoporous material is obtained.
Product structure of the present invention characterizes and performance evaluation：
Pass through the X-ray powder diffraction shown in accompanying drawing 1（XRD）Understand, attapulgite clay raw ore is 2θGo out at=8.41 °
Attapulgite is showed（001）Crystal face characteristic peak, but after hydro-thermal reaction formation analcime product, the characteristic peak of attapulgite is complete
Disappear, while the peak of quartz（2θ=26.8°）Also it is wholly absent, analcime occurs in the XRD curves of product（211）、
（400）With（332）Characteristic peak, illustrate that attapulgite clay and associated minerals are completely transformed into analcime, analcime purity is higher, knot
Brilliant degree is good.
Pass through the SEM shown in accompanying drawing 2（SEM）Understand, attapulgite clay is in Rod-like shape, rod crystalline substance beam
Assemble in bulk, and diameter about 20 has been obtained after hydro-thermal reactionµSilicate product spherical m.
By the pore size distribution curve shown in accompanying drawing 3, the pore-size distribution of attapulgite clay is divided into two regions：One
It is 10~25 nm macropore, two are distributed across the aperture in the range of 3.5~4.5 nm；After forming analcime, pore-size distribution is equal
One and integrated distribution in 3.5~4.5 nm, it is mesoporous material to illustrate the product to be formed.
By the attapulgite clay shown in accompanying drawing 4 and the absorption property curve of spherical analcime, attapulgite sticks
Native adsorbance only 138 mg/g to methylene blue, the analcime for recombinating formation are up to 198 mg/ to the adsorbance of methylene blue
g。
By the attapulgite clay shown in accompanying drawing 5 and the absorption property curve of spherical analcime, attapulgite sticks
Native adsorbance only 66.7 mg/g to tetracycline, the analcime for recombinating formation are up to 230.6 mg/g to the adsorbance of tetracycline.
By the attapulgite clay shown in accompanying drawing 6 and the absorption property curve of spherical analcime, attapulgite sticks
Native adsorbance only 75 mg/g to aureomycin, the analcime for recombinating formation are up to 295 mg/g to the adsorbance of tetracycline.
Claims (2)
1. the method for preparing spherical analcime mesoporous material using low-quality attapulgite clay mine tailing, it is characterised in that：It is by
Powder is made in the attapulgite clay mine tailing of low-quality, by solid-to-liquid ratio 1:60~1:6g/mL is distributed to changing containing 1 ~ 20% mass fraction
Property agent the aqueous solution in, then 1-12h is aged after being ultrasonically treated 65 min, is transferred in sealing hydro-thermal reaction tank, pressure 1.5 ~ 6
100 ~ 199 °C of MPa, temperature h of hydro-thermal reaction 4 ~ 100, product is separated, dried, crushes and obtains homogeneous spherical of pore-size distribution
Mesoporous analcime material；The modifying agent is sodium thiosulfate, sodium polysulfide, sodium sulfite, sodium hydrogensulfite, sodium sulphate, sulphur
Change sodium, sodium carbonate, sodium acid carbonate, potassium sulfide, potassium thiosulfate, potassium sulfite, potassium bisulfite, potassium sulfate, potassium carbonate, carbonic acid
At least one of hydrogen potassium, sodium metaaluminate, sodium hypochlorite, aluminium hydroxide.
2. the side according to claim 1 that spherical analcime mesoporous material is prepared using low-quality attapulgite clay mine tailing
Method, it is characterised in that：Described low-quality attapulgite clay mine tailing is low-grade ore and powder, and its chemical composition range is：
Al2O3,10.5% ~ 26%；MgO, 2.5% ~ 9%；SiO2,55% ~ 80%.
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| CN106809845A (en) * | 2017-04-11 | 2017-06-09 | 明光市安盛非金属材料厂 | A kind of method of modifying of attapulgite |
| CN107418587A (en) * | 2017-05-17 | 2017-12-01 | 郭迎庆 | A kind of preparation method of soil heavy metal combined passivator |
| CN108046289B (en) * | 2017-12-08 | 2020-10-16 | 昊青薪材（北京）技术有限公司 | Method for preparing potassium zeolite by using analcime powder |
| CN113288820B (en) * | 2021-05-25 | 2022-07-01 | 台州学院 | Organically modified attapulgite-dye hybrid pigment and preparation method and application thereof |
| CN114804134B (en) * | 2022-04-12 | 2023-07-25 | 中国科学院广州地球化学研究所 | Mesoporous material preparation method based on clay mineral |
| CN114918238A (en) * | 2022-05-07 | 2022-08-19 | 中国科学院生态环境研究中心 | Resistance heating process for enhancing multiphase extraction and repair effects of DNAPLS (deoxyribonucleic acid/liquid plastics) polluted site |
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| CN103572362A (en) * | 2013-01-11 | 2014-02-12 | 济南大学 | Method for hydrothermally synthesizing analcime monocrystal |
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Effective date of registration: 20210816 Address after: 730013 No.18 Tianshui Middle Road, Chengguan District, Lanzhou City, Gansu Province Patentee after: Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences Address before: 211700 No. 3 Dongfang Avenue, Xucheng Town, Xuyi county, Huai'an City, Jiangsu Province Patentee before: XUYI R & D CENTER FOR APPLICATION OF ATTAPULGITE CLAY, LANZHOU INSTITUTE OF CHEMICAL PHYSICS CHINESE ACADEMY OF SCIENCES |