CN108854941A - A kind of nanocomposite containing magnesium and preparation method thereof based on sepiolite preparation - Google Patents
A kind of nanocomposite containing magnesium and preparation method thereof based on sepiolite preparation Download PDFInfo
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- CN108854941A CN108854941A CN201810515394.2A CN201810515394A CN108854941A CN 108854941 A CN108854941 A CN 108854941A CN 201810515394 A CN201810515394 A CN 201810515394A CN 108854941 A CN108854941 A CN 108854941A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/12—Naturally occurring clays or bleaching earth
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28004—Sorbent size or size distribution, e.g. particle size
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
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Abstract
A kind of nanocomposite containing magnesium and preparation method thereof based on sepiolite preparation, first, sepiolite clay mineral are proportionally mixed with inorganic acid, stirring acidification a period of time under the conditions of certain temperature, secondly, aqueous slkali is added dropwise in acquired solution and adjusts its pH value, after continuing stirring, product is centrifuged, washing, it is dry to obtain product, the heavy metal pollution that can be effectively removed containing magnesium base composite material in environment of the silica support of the modified method preparation of the sepiolite mineral prepared through the invention, including rare earth Gd (III), traditional heavy metal Pb (II) and Cd (II) etc., with simple process, it can be mass-produced, the feature of Product environment close friend.
Description
Technical field
The present invention relates to technical field of nanometer material preparation, in particular to a kind of nanometer containing magnesium based on sepiolite preparation is multiple
Condensation material and preparation method thereof.
Background technique
Heavy metal refers to those with higher density, and the toxic or harmful metallic element under low concentration is a kind of
A series of problems, such as important environmental contaminants, their toxicity can cause ecology, nutrition, environment.Especially Pb (II), Hg
(II), Cd (II), Co (II), Ni (II), Cr (VI) etc., due to its toxicity and lethal effect, are listed in priority pollutant.
The existing method for handling heavy metal can be divided into biology and abiotic two class.The method of biology is based primarily upon plant
Enrichment with microorganism to heavy metal, abiotic method include such as precipitating, co-precipitation, ion exchange, solvent extraction, electricity
The physical and chemical processes such as solution, film filtering and absorption.Since plant and microorganism are the mistake of one long time-consuming to the enrichment of heavy metal
Journey, the abiotic physical chemistry removal means of heavy metal are still quickly to handle the important method of heavy metal at present.At these
In physico-chemical process, adsorption process is considered maximally efficient, economical, simple.
Clay bigger serface, price as possessed by it is low, be widely present soil and depositional environment in the advantages that, quilt
The heavy metal being widely used in removal water body.Clay goes the mechanism of removing heavy metals generally by ion-exchange reactions or a huge sum of money
Belong to and forms what inner-orbital complex was realized with ≡ Si-O- and ≡ the Al-O- group at clay particle edge.However, clay mineral exists
For in terms of heavy metal adsorption, itself intrinsic limitation, such as low load-carrying ability, relatively small metal bonding constant and right
The low selectivity of metal types limits its application in terms of heavy metal processing.
In order to solve above-mentioned limitation present in clay mineral, pass through ≡ Si-O- base possessed by clay mineral itself
Group reacts with the reagent containing special metal chelating function, to introduce new specific functional groups, in clay mineral with enhancing
Clay is studied the binding ability of heavy metal and the organically-modified of selectivity.However, clay mineral is to a huge sum of money after modification
The removal ability enhancing of category is not obvious.Also, organic reagent is generally required during carrying out organically-modified to clay
It helps, and process is complicated.
Sepiolite is a kind of typical layer chain clay, with the non-expansibility of bigger serface, light weight, it is porous, etc. spies
Point, has a wide range of applications.Acid processing is frequently used to increase the surface area of clay, to obtain with porous and active site
Solid material.In the sour treatment process of sepiolite, according to the intensity of acid, the Mg in sepiolite oxygen magnesium octahedron can be different
It removes to degree, in the case where the intensity of acid is sufficiently large, the amorphous SiO insoluble in acid can be formed2Gel.But due to sepiolite
The Mg that inside can be replaced with heavy metal cation2+It reduces, the Pb compared with sepiolite original sample, in acidification Wastewater on Sepiolite2+、
Cd2+、Sr2+、Co2+Etc. the adsorption efficiencies of heavy metal ion reduce instead.
Shepardite [Mg (OH)2] due to its environment friendly, high adsorption capacity and thermal stability, it is proved to be a kind of place
Manage heavy metal ion, such as Pb2+、Cu2+、Zn2+、Cd2+With the good inorganic agent of dyestuff.
Summary of the invention
In order to overcome the disadvantages of the above prior art, the purpose of the present invention is to provide a kind of containing based on sepiolite preparation
Magnesium nanocomposite and preparation method thereof, which can effectively remove the heavy metal pollution in environment, while have technique
Simplicity can be mass-produced, the feature of Product environment close friend.
In order to achieve the above object, the technical scheme adopted by the invention is as follows：
A kind of preparation method of the nanocomposite containing magnesium based on sepiolite preparation, steps are as follows：
Step 1：By sepiolite clay mineral and mass concentration be 2% inorganic acid according to solid-liquid mass ratio 1:10 mixing,
Stirring acidification 8-14h under the conditions of 50-80 DEG C of temperature；
Step 2：Aqueous slkali is added dropwise in step 1 acquired solution and adjusts its pH value greater than 9.5, continues to stir 0.5-2h
Afterwards, by product centrifugation, washing, dry acquisition product.
The content of scpiolitc is greater than 90% in the sepiolite clay mineral.
The sepiolite clay mineral are mechanically pulverized to less than 100 mesh powders.
The inorganic acid is one of hydrochloric acid, nitric acid or sulfuric acid.
The acidization condition of the sepiolite be 60 DEG C at a temperature of be stirred to react 12h.
The aqueous slkali is ammonium hydroxide or NaOH solution.
A kind of nanocomposite containing magnesium based on sepiolite preparation, product keep the original nano bar-shape knot of sepiolite
Structure, length are micron order scale, width 40-80nm.
The nanocomposite containing magnesium for heavy metal the heavy metals sun such as removal, including rare earth element, lead, cadmium from
Son.
The present invention having the beneficial effect that compared with prior art：
The present invention is by using the comprehensive continuous processing of Acid-Base to sepiolite clay, from sepiolite lattice in acidization
Then the magnesium ion of middle leaching carries out alkali process in situ, make in scpiolitc after by the integrated treatment of Acid-Base original position
Component recombinated and reacted, form the hydroxide of magnesium, during complete acidification, sepiolite be changed into have it is big
The silica amorphous of specific surface area greatly improves sepiolite to heavy metal sun to form novel nanocomposite
The removal capacity and removal efficiency of ion, and its capacity antacid is enhanced, also heavy metal ion is showed in acidic environment
Excellent removal ability out.The silica support of the modified method preparation of the sepiolite mineral prepared through the invention contains
Magnesium base composite material can effectively remove the heavy metal pollution in environment, including rare earth Gd (III), traditional heavy metal Pb (II)
With Cd (II) etc..Sepiolite feed distribution in the present invention is extensive, is easy to obtain, price economy, and preparation process is easy, can advise greatly
Mould production, Product environment are friendly, are the efficient passivation agent for controlling heavy metal pollution to heavy metals immobilization significant effect, have wide
Wealthy application prospect and market value.
Detailed description of the invention
Fig. 1 (a) is the TEM picture of scpiolitc；Fig. 1 (b) is the TEM picture for being acidified sepiolite；Fig. 1 (c) is soda acid
The TEM picture of sepiolite after processing.
Fig. 2 (a) is the EDX picture of scpiolitc；Fig. 2 (b) is the EDX picture for being acidified sepiolite；Fig. 2 c is at soda acid
The EDX picture of sepiolite after reason.
Fig. 3 is that sepiolite, the gained nanocomposite after acid-base integration is handled removes rare earth Gd (III) to pH value
Influence.
Fig. 4 (a) is sepiolite after acid-base integration processing to the removal ability curve graph of Gd (III)；Fig. 4 (b) is sepiolite
Removal ability curve graph of the sepiolite to Gd (III) after clay and sour modification.
Fig. 5 is that acid-base integration handles sepiolite under the conditions of low p H value to the removal capacity signal of rare earth Gd (III)
Figure.
Fig. 6 is that acid-base integration handles sepiolite to Pb2+And Cd2+Removal effect curve graph.
Specific embodiment
The present invention is described in further details below with reference to embodiment.
Embodiment 1 is based on sepiolite and prepares SiO2The nanocomposite containing magnesium of support
By sepiolite clay according to solid-to-liquid ratio 1:The ratio of 20 (mass ratioes), which is added in the hydrochloric acid that concentration is 5%, carries out acid
Change, 12h is stirred with the speed of 300r/min at 60 DEG C, ammonia spirit adjusting pH is then added dropwise in the above solution and arrives
9.5, with the speed stirring 2-3h of 300r/min at 60 DEG C, it is separated by solid-liquid separation, to get to based on sepiolite after washed and drying
The SiO of preparation2-Mg(OH)2Nanocomposite.
Carry out sample prepared by Acid-Base continuous processing in situ as former state to sepiolite original sample, acidification sepiolite and to sepiolite
The shape characteristic transmission electron microscope (TEM) of product is observed.Sepiolite shows a kind of typical fiber nano bar-shape structure as former state,
Length is micro-meter scale, width about 50nm, referring to Fig. 1 (a).Energy spectrum analysis (EDX) discovery club shaped structure sepiolite contain O,
These three elements of Si, Mg, referring to fig. 2 (a).Club shaped structure, but fiber are still shown after the acidified processing of sepiolite original sample
The gap of bar-like inner increased significantly, referring to Fig. 1 (b).Energy spectrum analysis is found, Mg element is no longer contained in sample, referring to fig. 2
(b).The result shows that acid, which is handled, destroys the octahedral structure of oxygen magnesium in sepiolite crystal, and more stable oxygen-octahedron
It is retained, forms silicon dioxide colloid.Referring to Fig. 1 (c), for sepiolite original sample institute after peracid and ammonium hydroxide original position continuous processing
The transmission photo for obtaining sample shows that sample generates a kind of new nanometer therefrom it can be found that rodlike surface becomes more coarse
Composite material, energy spectrum analysis find the presence for having Mg element in product, referring to fig. 2 (c), show sepiolite former by Acid-Base
A kind of novel SiO is formd after the integrated treatment of position2-Mg(OH)2Nanocomposite.
Clay used in the embodiment of the present invention is the sepiolite clay mineral in sepiolite group, is pushed away according to reaction principle
It is disconnected, when using other clay mineral attapulgite hybrids of sepiolite group, it can also reach technical effect of the invention.
PH value is as follows to the impact analysis of nanocomposite removal rare earth Gd (III)：
It takes the nanocomposite containing magnesium prepared in example 1 0.1g to be respectively placed in 100mL and 0.1mmol/L is housed (about
15.1mg/L) in the solution of Gd (III), pH research range is set as 3.0 to 7.5, (25 DEG C) stirring 12h of constant temperature.
Gd (III) can almost be completely removed within the scope of an extensive pH by composite material as can see from Figure 3,
It is not influenced by the initial pH of solution.For sepiolite original sample and amorphous SiO2For, they are to the removal rate of Gd (III) selected
It takes lower than composite material within the scope of pH, and increases with pH and increase, show to be more advantageous to amorphous SiO under high ph conditions2It is right
The removal of Gd (III).SiO2-Mg(OH)2Composite material shows the removal ability excellent to Gd (III) within the scope of wide pH value,
This may be related with the aobvious alkalinity of shepardite dissolution, and shepardite dissolution increases solution ph, to keep adsorbent surface negatively charged
Lotus is more advantageous to the removal to Gd (III).
Nanocomposite based on sepiolite preparation is as follows to the removal capacity analysis of Gd (III)：
The nanocomposite containing magnesium prepared in example 1 0.1g is taken to be respectively placed in 100mL molten equipped with various concentration Gd (III)
In the beaker of liquid, it is 0.1-6mmol/L, under conditions of neutral ph, (25 DEG C) stirring 12h of constant temperature that range, which is arranged, in concentration.To Hai Pao
Stone carries out simple Acid-Base mixed processing in situ SiO prepared later2-Mg(OH)2Removal of the nanocomposite to Gd (III)
Capacity is up to 4.45mmol/g (703.1mg/g), and referring to fig. 4 (a), and sepiolite is to the removal capacity of Gd (III)
0.159mmol/g (25.12mg/g) is acidified the amorphous SiO of sepiolite preparation completely2Removal capacity to Gd (III) is only
0.066mmol/g (10.43mg/g) referring to fig. 4 (b), as a result illustrates after being modified to sepiolite prepared nano combined
Material significantly promotes the removal capacity of rare earth Gd (III), is sepiolite as former state to the 28 of Gd (III) processing capacity
Times, with the amorphous SiO obtained after acidification sepiolite2It compares, even more improves nearly 67 times.
Nanocomposite based on sepiolite preparation is as follows to the removal capacity analysis of Gd (III) at various ph values：
The nanocomposite containing magnesium prepared in example 1 0.1g is taken to be respectively placed in 100mL molten equipped with various concentration Gd (III)
In the beaker of liquid, it is 0.1-6mmol/L that range, which is arranged, in concentration, while adjusting pH value to 3 or 5, (25 DEG C) stirring 12h of constant temperature.It is multiple
It is 3.52 and 4.1mmol/g to the removal capacity of Gd (III) under the conditions of pH 3.0 and 5.0 to condensation material, referring to figure (5).
The result shows that the modified prepared composite material of sepiolite has good Antacid effectiveness, in low ph value
Under the conditions of, rare earth Gd (III) is still shown greatly to remove capacity.
Nanocomposite based on sepiolite preparation is to Pb2+And Cd2+Removal effect be analyzed as follows：
The nanocomposite containing magnesium prepared in example 1 0.1g is taken to be respectively placed in 100m L equipped with various concentration Pb2+And Cd2 +In the beaker of solution, it is 0.1-6mmol/L that range, which is arranged, in concentration, while adjusting pH value to 5.6. the results show that based on sepiolite
The SiO of preparation2-Mg(OH)2Nanocomposite is to Pb2+And Cd2+Removal capacity respectively be up to 6.8mmol/g (about 1400mg/
G) and 4.8mmol/g (about 550mg/g) is referring to figure (6), after carrying out simple Acid-Base processing to sepiolite, to tradition weight
Metal Pb2+And Cd2+Removal capacity greatly improve.
Claims (9)
1. a kind of preparation method of the nanocomposite containing magnesium based on sepiolite preparation, which is characterized in that include the following steps：
Step 1：By sepiolite clay mineral and mass concentration be 2% inorganic acid according to solid-liquid mass ratio 1:10 mixing, in 50-
Stirring acidification 8-14h under the conditions of 80 DEG C of temperature；
Step 2：Aqueous slkali is added dropwise in step 1 acquired solution and adjusts its pH value greater than 9.5, continues after stirring 0.5-2h,
By product centrifugation, washing, dry acquisition product.
2. a kind of preparation method of the nanocomposite containing magnesium based on sepiolite preparation, feature according to claim
It is, the content of scpiolitc is greater than 90% in the sepiolite clay mineral.
3. a kind of preparation method of the nanocomposite containing magnesium based on sepiolite preparation, feature according to claim
It is, the sepiolite clay mineral are mechanically pulverized to less than 100 mesh powders.
4. a kind of preparation method of the nanocomposite containing magnesium based on sepiolite preparation, feature according to claim
It is, the inorganic acid is one of hydrochloric acid, nitric acid or sulfuric acid.
5. a kind of preparation method of the nanocomposite containing magnesium based on sepiolite preparation, feature according to claim
Be, the acidization condition of the sepiolite be 60 DEG C at a temperature of be stirred to react 12h.
6. a kind of preparation method of the nanocomposite containing magnesium based on sepiolite preparation, feature according to claim
It is, the aqueous slkali is ammonium hydroxide or NaOH solution.
What 7. a kind of preparation method of the nanocomposite containing magnesium based on sepiolite preparation as described in claim 1 was prepared
Nanocomposite containing magnesium.
8. nanocomposite containing magnesium according to claim 7, which is characterized in that the nanocomposite containing magnesium keeps sea
The original nano bar-shape structure of afrodite, length are micron order scale, width 40-80nm.
9. nanocomposite containing magnesium according to claim 7, which is characterized in that the nanocomposite containing magnesium is for weight
The heavy metal cations such as the removal of metal, including rare earth element, lead, cadmium.
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| CN110075789A (en) * | 2019-05-23 | 2019-08-02 | 陕西科技大学 | A kind of cyanobacteria magnetic based on the modified preparation of attapulgite catches the preparation method of agent |
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| CN110550723A (en) * | 2019-09-04 | 2019-12-10 | 湖南宇山玉月农业科技有限公司 | Biological filler for treating livestock and poultry wastewater |
| CN111320984A (en) * | 2020-04-21 | 2020-06-23 | 江苏省地质调查研究院 | Farmland heavy metal contaminated soil passivator and preparation method and application thereof |
| CN111514845A (en) * | 2020-04-15 | 2020-08-11 | 大连理工大学 | CO based on natural clay2Adsorbent and preparation method thereof |
| CN112111977A (en) * | 2020-07-28 | 2020-12-22 | 浙江锶通净新材料有限公司 | Flame-retardant transition metal oxide sepiolite composite material, and preparation method and application thereof |
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| CN110075789A (en) * | 2019-05-23 | 2019-08-02 | 陕西科技大学 | A kind of cyanobacteria magnetic based on the modified preparation of attapulgite catches the preparation method of agent |
| CN110237804A (en) * | 2019-07-18 | 2019-09-17 | 陕西科技大学 | A kind of method and application preparing efficient phosphorus adsorbent with asbestos tailings |
| CN110550723A (en) * | 2019-09-04 | 2019-12-10 | 湖南宇山玉月农业科技有限公司 | Biological filler for treating livestock and poultry wastewater |
| CN111514845A (en) * | 2020-04-15 | 2020-08-11 | 大连理工大学 | CO based on natural clay2Adsorbent and preparation method thereof |
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| CN112111977B (en) * | 2020-07-28 | 2022-08-05 | 浙江锶通净新材料有限公司 | Flame-retardant transition metal oxide sepiolite composite material, and preparation method and application thereof |
| CN112934168A (en) * | 2021-02-08 | 2021-06-11 | 浙江工业大学 | Magnesium-containing silica gel composite material and preparation method and application thereof |
| CN115318287A (en) * | 2021-12-16 | 2022-11-11 | 中国科学院大连化学物理研究所 | Catalyst for preparing styrene by toluene side chain alkylation and preparation method and application thereof |
| CN115318287B (en) * | 2021-12-16 | 2024-03-19 | 中国科学院大连化学物理研究所 | Catalyst for preparing styrene by toluene side chain alkylation and preparation method and application thereof |
| CN114768750A (en) * | 2022-05-05 | 2022-07-22 | 中南大学 | Method for preparing iron-based layered double hydroxide arsenic removal adsorbent from red mud |
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