CN108671896A - A kind of modified montmorillonite used and preparation method thereof, heavy metal chelating agent - Google Patents
A kind of modified montmorillonite used and preparation method thereof, heavy metal chelating agent Download PDFInfo
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- CN108671896A CN108671896A CN201810487008.3A CN201810487008A CN108671896A CN 108671896 A CN108671896 A CN 108671896A CN 201810487008 A CN201810487008 A CN 201810487008A CN 108671896 A CN108671896 A CN 108671896A
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
Abstract
A kind of modified montmorillonite used and preparation method thereof, heavy metal chelating agent, the invention belongs to modified montmorillonite used preparing technical fields.Amino acid hydrochloride salt is added into montmorillonite suspension, the suspension is then tuned into faintly acid, depressurizes and filters after stirring, dried after washing, ground, is obtained after sieve of looking over so as to check modified montmorillonite used.It is obtained by the reaction with amino acid hydrochloride salt by montmorillonite under mildly acidic conditions modified montmorillonite used, can effectively increase interlamellar spacing by modified montmorillonite, to improve its adsorption capacity.
Description
Technical field：
The invention belongs to modified montmorillonite used preparing technical fields, in particular to a kind of modified montmorillonite used and its preparation side
Method, heavy metal chelating agent.
Background technology：
In the industrial processes such as plating processing, mining, battery manufacture, along with the production of heavy metal contaminants
It is raw and and its phenomenon that pollution environment, heavy metal ion cannot be biodegradable, and the last intoxicating of biological accumulation can occurs in it
Or it is carcinogenic.The method of common heavy metal chelating agent has chemical precipitation method, ion-exchange, absorption method and electrochemical treatments technology
Deng.These methods have respective characteristics and available field, some methods are often because of high cost, poor feasibility and there is secondary pollutions
Problem and cannot be widely used.Wherein absorption method is attracted people's attention because easy to operate and effect is good.
For montmorillonite because its cationic cross-over value is high, adsorption effect is good, abundant raw material, at low cost and environmental-friendly and extensive
Using.Its main active is montmorillonite, is that two layers of oxygen-octahedron clips one layer of alumina octahedral in structure.Due to
Isomorphous substitution (the Al between such as octahedral layer3+By Mg2+Or Fe2+It replaces, the Si between tetrahedral layer4+By Al3+Displacement etc.), interlayer
There is superfluous negative electrical charge, these superfluous negative electrical charges attract the Na between montmorillonite layer by electrostatic interaction+And Ca2+Reach electrostatic equilibrium.
It, can be by other cationic (including inorganic cations and organic since these cations are weaker with the binding force of montmorillonite lamella
Cation) it exchanges again.But natural smectite, because active site is occupied, adsorption efficiency is low.
Invention content
It is an object of the present invention to providing a kind of modified montmorillonite used preparation method in view of the deficiencies of the prior art, lead to
Cross montmorillonite under mildly acidic conditions be obtained by the reaction with amino acid hydrochloride salt it is modified montmorillonite used.
The second object of the present invention is to provide a kind of modified montmorillonite used, can effectively increase by modified montmorillonite
Interlamellar spacing, to improve its adsorption capacity.
The third object of the present invention is to provide a kind of heavy metal chelating agent.
In order to realize that the above-mentioned purpose of the present invention, spy use following technical scheme：
A kind of modified montmorillonite used preparation method, including：It is to be modified with group amino acid hydrochloride salt using montmorillonite as raw material
Agent is modified montmorillonite.
Preferably, modification carries out in the following manner：Montmorillonite suspension is mixed with amino acid hydrochloride salt, then will be covered de-
Stone suspension is tuned into acidity, depressurizes and filters after stirring, dried after washing, is ground, and is obtained after sieve of looking over so as to check modified montmorillonite used.
Preferably, montmorillonite suspension obtains in the following manner：Montmorillonite is mixed with deionized water, stirs, illiteracy is made
De- stone suspension；
Preferably, montmorillonite is na-montmorillonite；
Preferably, na-montmorillonite and deionized water solid-to-liquid ratio 1:50-100.
Preferably, the amount of amino acid hydrochloride salt is the 80-100% of cation exchange capacity in montmorillonite suspension；It covers de-
The cation exchange capacity of stone is 80-100mmoL/100g.
Preferably, the pH of montmorillonite suspension is 4-5.
Preferably, stirring is to stir 12-24h under 20-60 DEG C of water bath condition.
Preferably, drying temperature is 60-80 DEG C.
Preferably, the screen size of mesh sieve is 53-75 μm.
It is a kind of modified montmorillonite used, it is obtained prepared by the preparation method by any of the above-described.
A kind of heavy metal chelating agent includes above-mentioned modified montmorillonite used.
Compared with prior art, the invention has the advantages that：
1. reaction condition of the present invention is simple, reaction process is simply easily operated.Reaction carries out in aqueous solution, environment friend
It is good.
2. raw material of the present invention is natural minerals, raw material sources are abundant, at low cost and nontoxic, are convenient for industrialized production.
3. the modifying agent group amino acid hydrochloride salt selected by the present invention is a kind of amino-acid salt containing imidazolyl groups, it is inserted into
After between montmorillonite layer, the heavy metal ion such as Pb, Cu in adsorbent solution can make heavy metal ion and the N atom knots on imidazole radicals
Conjunction forms complex, keeps absorption more secured, is not easy to be desorbed, and adsorption efficiency is high, is expected to realize permanent absorption.
Specific implementation mode
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will
Understand, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the invention.It is not specified in embodiment specific
Condition person carries out according to conventional conditions or manufacturer's recommended conditions.Reagents or instruments used without specified manufacturer is
The conventional products that can be obtained by commercially available purchase.
Based on the crosslinking of micro content oxygen catalytic prepared by modified montmorillonite used preparation to a kind of of the embodiment of the present invention below
Method is specifically described.
As one aspect of the present invention, the present invention provides a kind of modified montmorillonite used preparation method, include mainly with
Lower step：Amino acid hydrochloride salt is added into montmorillonite suspension, suspension is then tuned into faintly acid, depressurizes and takes out after stirring
Filter, is dried after washing, is ground, and is obtained after sieve of looking over so as to check modified montmorillonite used.
Preferably, montmorillonite suspension obtains in the following manner：Montmorillonite is mixed with deionized water, is stirred at 0-40 DEG C
10-30min is mixed, montmorillonite suspension is made；Such as in the embodiment of the present invention whipping temp could be provided as 0 DEG C, 10 DEG C, 20
DEG C, 30 DEG C, 40 DEG C, such as in the embodiment of the present invention mixing time could be provided as 10min, 15min, 20min, 25min,
30min。
Preferably, montmorillonite is na-montmorillonite；Although other montmorillonites also can be used as it is modified montmorillonite used, for weight
Metal trapping effect can not show a candle to na-montmorillonite, therefore the present invention preferably montmorillonite is na-montmorillonite.
Preferably, na-montmorillonite and deionized water solid-to-liquid ratio 1:50-100.Such as sodium base covers in the embodiment of the present invention
De- stone could be provided as 1 with deionized water solid-to-liquid ratio:50、1:60、1:70、1:80、1:90、1:100.
Preferably, the screen size of mesh sieve is 200 mesh, 230 mesh, 270 mesh.The size of 200 mesh is≤75 μm, 230 purposes
Size is≤63 μm, and the size of 270 mesh is≤53 μm.Such as the screen size that mesh sieves in the embodiment of the present invention could be provided as
200 mesh, 230 mesh, 270 mesh.
Preferably, the amount of the amino acid hydrochloride salt of addition is the 80-100% of cation exchange capacity in montmorillonite suspension
The ratio of CEC.The ratio of the 80%CEC of cation exchange capacity i.e. the ratio of 90%CEC be also in montmorillonite suspension
It is that 4g montmorillonites are mixed with 0.675g amino acid hydrochloride salts, the ratio of the 100%CEC of cation exchange capacity in montmorillonite suspension
Example i.e. 4g montmorillonites are mixed with 0.75g amino acid hydrochloride salts.
Preferably, weakly acidic pH=4-5.Such as in the embodiment of the present invention weakly acidic pH could be provided as 4,4.5,
5。
Preferably, the CEC of montmorillonite is 80-100mmoL/100g.
Preferably, stirring stirs 12-24h under 20-60 DEG C of water bath condition.Such as the water stirred in the embodiment of the present invention
Bath temperature is set as 20 DEG C, 30 DEG C, 40 DEG C, 50 DEG C, 60 DEG C, such as the stirring in water bath time is set as in the embodiment of the present invention
12h、15h、18h、21h、24h。
Preferably, drying temperature is 60-80 DEG C.Such as in the embodiment of the present invention drying temperature be set as 60 DEG C, 65 DEG C,
70℃、75℃、80℃。
As two aspects of the present invention, present invention offer is a kind of modified montmorillonite used, by the preparation method of any of the above-described
It is prepared to obtain, it can effectively increase interlamellar spacing by modified montmorillonite, to improve its adsorption capacity.
As three aspects of the present invention, the present invention provides a kind of heavy metal chelating agent by above-mentioned modified montmorillonite used system
At, heavy metal chelating agent for including Pb, Cu etc. toxic heavy metals ion play the role of good trapping and absorb.
Adsorbance calculation formula is as follows in the present invention：
In formula：
qe：Heavy metal ion adsorbed capacity, unit mg/g；
C0：Heavy metal ion initial concentration, unit mg/L；
Ce：Heavy metal ion adsorbed equilibrium concentration, unit mg/L；
V：Liquor capacity, unit L；
m：Adsorbent mass, unit g.
Removal rate calculation formula is as follows in the present invention：
η：Removal rate (%)
C0：Heavy metal ion initial concentration, unit mg/L；
Ce：Heavy metal ion adsorbed equilibrium concentration, unit mg/L；
V：Liquor capacity, unit L；
Embodiment 1
1. 4g na-montmorillonites are distributed in 200mL deionized waters, 10min is stirred at 0 DEG C.It is added into the suspension
0.60g group amino acid hydrochloride salts adjust the pH=5 of suspension with 1MHCl.It stirs for 24 hours, filters, 80 under 20 DEG C of water bath conditions
DEG C drying, grinding, cross 200 mesh sieve, you can obtain modified montmorillonite used.
2. weighing, 0.1g is above-mentioned modified montmorillonite used, puts into the Pb solution that 100mL initial concentrations are 100mg/L, pH=
5.90min is stirred at 25 DEG C, after centrifugation, measures the residual concentration of Pb in supernatant.The result shows that modified montmorillonite used right
The adsorbance of Pb (II) is 63.25mg/g, removal rate 63.25%.
Embodiment 2
1. 4g na-montmorillonites are distributed in 240mL deionized waters, 15min is stirred at 10 DEG C.Add into the suspension
Enter 0.60g group amino acid hydrochloride salts, the pH=4.5 of suspension is adjusted with 1M HCl.21h is stirred under 30 DEG C of water bath conditions, is taken out
Filter, 75 DEG C of drying, grinding cross 230 mesh sieve, you can obtain modified montmorillonite used.
2. weigh it is modified montmorillonite used in 0.1g examples detailed above 1, put into 100mL initial concentrations be 25mg/L Cu (II) it is molten
In liquid, pH=5.90min is stirred under 25 DEG C of water bath conditions, after centrifugation, measures the residual concentration of Cu (II) in supernatant.
The result shows that the modified montmorillonite used adsorbance to Cu (II) is 18.39mg/g, removal rate 73.56%.
Embodiment 3
1. 4g na-montmorillonites are distributed in 280mL deionized waters, 20min is stirred at 20 DEG C.Add into the suspension
Enter 0.675g group amino acid hydrochloride salts, the pH=5.0 of suspension is adjusted with 1M HCl.18h is stirred under 40 DEG C of water bath conditions, is taken out
Filter, 70 DEG C of drying, grinding cross 270 mesh sieve, you can obtain modified montmorillonite used.
2. weighing, 0.1g is above-mentioned modified montmorillonite used, puts into the Pb solution that 100mL initial concentrations are 100mg/L, pH=
5.80min is stirred at 30 DEG C, after centrifugation, measures the residual concentration of Pb in supernatant.The result shows that modified montmorillonite used right
The adsorbance of Pb is 61.12mg/g, removal rate 61.12%.
Embodiment 4
1. 4g na-montmorillonites are distributed in 320mL deionized waters, 15min is stirred at 30 DEG C.Add into the suspension
Enter 0.675g group amino acid hydrochloride salts, the pH=4.0 of suspension is adjusted with 1M HCl.15h is stirred under 50 DEG C of water bath conditions, is taken out
Filter, 65 DEG C of drying, grinding cross 200 mesh sieve, you can obtain modified montmorillonite used.
2. weighing, 0.1g is modified montmorillonite used, puts into the Cu solution that 100mL initial concentrations are 25mg/L, pH=4.20
100min is stirred under DEG C water bath condition, after centrifugation, measures the residual concentration of Cu in supernatant.The result shows that modified cover takes off
Stone is 17.57mg/g, removal rate 70.28% to the adsorbance of Cu.
Embodiment 5
1. 4g na-montmorillonites are distributed in 360mL deionized waters, 10min is stirred at 40 DEG C.Add into the suspension
Enter 0.75g group amino acid hydrochloride salts, the pH=4.5 of suspension is adjusted with 1M HCl.12h is stirred under 60 DEG C of water bath conditions, is taken out
Filter, 60 DEG C of drying, grinding cross 230 mesh sieve, you can obtain modified montmorillonite used.
2. weighing, 0.1g is above-mentioned modified montmorillonite used, puts into the Pb solution that 100mL initial concentrations are 200mg/L, pH=
4.5.80min is stirred at 40 DEG C, after centrifugation, measures the residual concentration of Pb in supernatant.The result shows that modified montmorillonite used
Adsorbance to Pb is 85.60mg/g, removal rate 42.80%.
Embodiment 6
1. 4g na-montmorillonites are distributed in 400mL deionized waters, 20min is stirred at 20 DEG C.Add into the suspension
Enter 0.60g group amino acid hydrochloride salts, the pH=5.0 of suspension is adjusted with 1M HCl.18h is stirred under 40 DEG C of water bath conditions, is taken out
Filter, 70 DEG C of drying, grinding cross 200 mesh sieve, you can obtain modified montmorillonite used.
2. weighing, 0.1g is modified montmorillonite used, puts into the Cu solution that 100mL initial concentrations are 50mg/L, pH=5.0.
90min is stirred under 25 DEG C of water bath conditions, after centrifugation, measures the residual concentration of Cu in supernatant.The result shows that modified cover takes off
Stone is 24.01mg/g, removal rate 48.02% to the adsorbance of Cu.
Embodiment 7
1. 4g na-montmorillonites are distributed in 200mL deionized waters, 10min is stirred at 0 DEG C.It is added into the suspension
0.60g group amino acid hydrochloride salts adjust the pH=5 of suspension with 1MHCl.It stirs for 24 hours, filters, 80 under 20 DEG C of water bath conditions
DEG C drying, grinding, cross 200 mesh sieve, you can obtain modified montmorillonite used.
2. weighing, 0.1g is above-mentioned modified montmorillonite used, puts into the Pb solution that 100mL initial concentrations are 300mg/L, pH=
5.90min is stirred at 25 DEG C, after centrifugation, measures the residual concentration of Pb in supernatant.The result shows that modified montmorillonite used right
The adsorbance of Pb is 107.67mg/g, removal rate 35.89%.
Embodiment 8
1. 4g na-montmorillonites are distributed in 240mL deionized waters, 15min is stirred at 10 DEG C.Add into the suspension
Enter 0.60g group amino acid hydrochloride salts, the pH=4.5 of suspension is adjusted with 1M HCl.21h is stirred under 30 DEG C of water bath conditions, is taken out
Filter, 75 DEG C of drying, grinding cross 230 mesh sieve, you can obtain modified montmorillonite used.
2. weigh it is modified montmorillonite used in 0.1g examples detailed above 1, put into 100mL initial concentrations be 75mg/L Cu (II) it is molten
In liquid, pH=4.5.90min is stirred under 25 DEG C of water bath conditions, after centrifugation, measures the residual concentration of Cu in supernatant.Knot
Fruit shows that the modified montmorillonite used adsorbance to Cu is 30.72mg/g, removal rate 40.96%.
Embodiment 9
1. 4g na-montmorillonites are distributed in 280mL deionized waters, 20min is stirred at 20 DEG C.Add into the suspension
Enter 0.675g group amino acid hydrochloride salts, the pH=5.0 of suspension is adjusted with 1M HCl.18h is stirred under 40 DEG C of water bath conditions, is taken out
Filter, 70 DEG C of drying, grinding cross 270 mesh sieve, you can obtain modified montmorillonite used.
2. weighing, 0.1g is above-mentioned modified montmorillonite used, puts into the Pb solution that 100mL initial concentrations are 400mg/L, pH=
5.80min is stirred at 30 DEG C, after centrifugation, measures the residual concentration of Pb in supernatant.The result shows that modified montmorillonite used right
The adsorbance of Pb is 110.2mg/g, removal rate 27.55%.
Embodiment 10
1. 4g na-montmorillonites are distributed in 320mL deionized waters, 15min is stirred at 30 DEG C.Add into the suspension
Enter 0.675g group amino acid hydrochloride salts, the pH=4.0 of suspension is adjusted with 1M HCl.15h is stirred under 50 DEG C of water bath conditions, is taken out
Filter, 65 DEG C of drying, grinding cross 200 mesh sieve, you can obtain modified montmorillonite used.
2. weighing, 0.1g is modified montmorillonite used, puts into the Cu solution that 100mL initial concentrations are 100mg/L, pH=4.
100min is stirred under 20 DEG C of water bath conditions, after centrifugation, measures supernatant 31.18mg/g, removal rate 31.18%.
Embodiment 11
1. 4g na-montmorillonites are distributed in 360mL deionized waters, 10min is stirred at 40 DEG C.Add into the suspension
Enter 0.75g group amino acid hydrochloride salts, the pH=4.5 of suspension is adjusted with 1M HCl.12h is stirred under 60 DEG C of water bath conditions, is taken out
Filter, 60 DEG C of drying, grinding cross 230 mesh sieve, you can obtain modified montmorillonite used.
2. weighing, 0.1g is above-mentioned modified montmorillonite used, puts into the Pb solution that 100mL initial concentrations are 500mg/L, pH=
4.5.80min is stirred at 40 DEG C, after centrifugation, measures the residual concentration of Pb in supernatant.The result shows that modified montmorillonite used
Adsorbance to Pb is 113.6mg/g, removal rate 22.72%.
Embodiment 12
1. 4g na-montmorillonites are distributed in 400mL deionized waters, 20min is stirred at 20 DEG C.Add into the suspension
Enter 0.60g group amino acid hydrochloride salts, the pH=5.0 of suspension is adjusted with 1M HCl.18h is stirred under 40 DEG C of water bath conditions, is taken out
Filter, 70 DEG C of drying, grinding cross 200 mesh sieve, you can obtain modified montmorillonite used.
2. weighing, 0.1g is modified montmorillonite used, puts into the Cu solution that 100mL initial concentrations are 125mg/L, pH=5.0.
90min is stirred under 25 DEG C of water bath conditions, after centrifugation, measures the residual concentration of Cu in supernatant.The result shows that modified cover
De- stone is 31.8mg/g, removal rate 25.44% to the adsorbance of Cu.
Compared with prior art, the present invention having following remarkable advantage：
1. reaction condition of the present invention is simple, easily operated.Reaction carries out in aqueous solution, environmental-friendly.
2. raw material of the present invention is natural minerals, raw material sources are abundant, at low cost and nontoxic, are convenient for industrialized production.
It is a kind of amino-acid salt containing imidazolyl groups 3. the modifying agent selected by the present invention is amino acid hydrochloride salt, inserts
After entering between montmorillonite layer, the heavy metal ion such as Pb, Cu in adsorbent solution can make heavy metal ion and the N atoms on imidazole radicals
In conjunction with complex is formed, keep absorption more secured, be not easy to be degraded and be desorbed, adsorption efficiency is high, is expected to realize permanent absorption.
Although illustrate and describing the present invention with specific embodiment, it will be appreciated that without departing substantially from the present invention's
Many other change and modification can be made in the case of spirit and scope.It is, therefore, intended that wrapping in the following claims
Include all such changes and modifications belonged in the scope of the invention.
Claims (10)
1. a kind of modified montmorillonite used preparation method, which is characterized in that including：Using montmorillonite as raw material, with a group amino acid hydrochloric acid
Salt is modifying agent, is modified to montmorillonite.
2. a kind of modified montmorillonite used preparation method according to claim 1, which is characterized in that the modification is by following
Mode carries out：The montmorillonite suspension is mixed with the amino acid hydrochloride salt, it is then that the montmorillonite is suspended
Liquid is tuned into acidity, depressurizes and filters after stirring, dried after washing, is ground, and is obtained after sieve of looking over so as to check modified montmorillonite used.
3. a kind of modified montmorillonite used preparation method according to claim 2, which is characterized in that the montmorillonite is suspended
Liquid obtains in the following manner：The montmorillonite is mixed with deionized water, stirs, montmorillonite suspension is made；
Preferably, the montmorillonite is na-montmorillonite；
Preferably, the na-montmorillonite and the deionized water solid-to-liquid ratio 1:50-100.
4. a kind of modified montmorillonite used preparation method according to claim 2, which is characterized in that the amino acid hydrochloric acid
The amount of salt is the 80-100% of cation exchange capacity in the montmorillonite suspension；The cation of the montmorillonite exchanges
Capacity is 80-100mmoL/100g.
5. a kind of modified montmorillonite used preparation method according to claim 2, which is characterized in that the montmorillonite is suspended
The pH of liquid is 4-5.
6. a kind of modified montmorillonite used preparation method according to claim 2, which is characterized in that the stirring be
12-24h is stirred under 20-60 DEG C of water bath condition.
7. a kind of modified montmorillonite used preparation method according to claim 2, which is characterized in that the drying temperature is
60-80℃。
8. a kind of modified montmorillonite used preparation method according to claim 2, which is characterized in that the sieve pore of the mesh sieve
Size is 53-75 μm.
9. it is a kind of modified montmorillonite used, it is obtained prepared by claim 1-8 any one of them preparation methods.
10. a kind of heavy metal chelating agent includes modified montmorillonite used described in claim 9.
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| CN115382502A (en) * | 2022-08-22 | 2022-11-25 | 南京植创生物技术研究院有限公司 | Preparation method of glycyrrhiza triterpenoid glycoside silicate montmorillonite complex, complex and application thereof |
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| CN112655823A (en) * | 2020-12-04 | 2021-04-16 | 淮阴工学院 | Clay/amino acid compound additive and preparation method and application thereof |
| CN112655823B (en) * | 2020-12-04 | 2024-01-23 | 淮阴工学院 | Clay/amino acid compound additive and preparation method and application thereof |
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