CN106984364A - Application of the SAPO molecular sieve analog original powder in separated/extracted metal ion - Google Patents
Application of the SAPO molecular sieve analog original powder in separated/extracted metal ion Download PDFInfo
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J39/00—Cation exchange; Use of material as cation exchangers; Treatment of material for improving the cation exchange properties
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- B01J39/12—Compounds containing phosphorus
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- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/26—Selective adsorption, e.g. chromatography characterised by the separation mechanism
- B01D15/36—Selective adsorption, e.g. chromatography characterised by the separation mechanism involving ionic interaction
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Abstract
This application discloses application of the former powder of SAPO molecular sieve analog in Selective Separation/extraction metal ion, using the former powder of SAPO molecular sieve analog, the some metal ions of selective exchange adsorption in mixing salt solution, the relative separation of metal salt is realized by the means of phase transfer.The use of molecular screen primary powder alternatively property ion-exchanger, opens the frontier of ion exchange material；Molecular screen material species is abundant, various structures, it is contemplated that by selecting suitable topological structure, port size and Template Types, ion selectivity and segregation ratio to former powder molecular sieve regulate and control.
Description
Technical field
The application is related to a kind of specific ion exchanger, belongs to separating-purifying field.
Background technology
Nineteen eighty-two, U.S. combinating carbide company successfully develops a series of aluminium phosphate molecular sieves and its spread out
Biology (Pat：USP 4310440, USP 4,440,871), henceforth, aluminium phosphate molecular sieve and its
Heterosubstituted derivatives are constantly subjected to extensive concern, are material science and the research heat of catalytic field
Point.Especially SAPO-n (n is model) series silicoaluminophosphamolecular molecular sieves：Its skeleton is by PO2 +、AlO2 -
And SiO2Tetrahedron is constituted, and Si atoms substitution Al atoms enter neutral aluminium phosphate molecular sieve skeleton, make
Generation skeleton negative electrical charge.By different and Si contents the differences of synthesis condition, SAPO molecular sieve is presented
To strong Bronsted acidity in, many SAPO molecular sieves have well-regulated pore passage structure and good in addition
Good heat endurance and hydrothermal stability, such material have been widely used as adsorbent, catalyst and urged
Agent carrier, is paid much attention to by domestic and international academia and industrial quarters.But SAPO molecular sieve analogs
Organic formwork agent is used mostly in building-up process, the former powder molecular sieve pore passage and cavity of synthesis are by template
Occupied by agent, calcination process is typically all first carried out before the use, removes the organic formwork wherein contained
Agent, so that duct is unimpeded, if subsequently to carry out ion exchange process, typically can first be exchanged for NH4 +
Type, then carry out ion exchange with other ions.
Colored metallurgical industrial gives off a large amount of waste water, is the main source of water body metal, Metallurgical Waste Water into
Divide complexity, pollutant load is high, directly outer arrange can cause very big pollution, therefore Metallurgical Waste Water to environment
Processing and recycle tool have very important significance.
The content of the invention
According to the one side of the application there is provided the former powder of SAPO molecular sieve analog in Selective Separation
Application in/extraction metal ion, using the former powder of SAPO molecular sieve analog, in mixing salt solution
The some metal ions of exchange adsorption of selectivity, relative point of metal salt is realized by the means of phase transfer
From.The use of molecular screen primary powder alternatively property ion-exchanger, opens the new of ion exchange material
Field；Molecular screen material species is abundant, various structures, it is contemplated that by selecting suitable topological structure,
Port size and Template Types, ion selectivity and segregation ratio to former powder molecular sieve are adjusted
Control.
Application of the former powder of the SAPO molecular sieve analog in Selective Separation/extraction metal ion,
Characterized in that, the former powder of the SAPO molecular sieve analog is the SAPO containing organic formwork agent
Molecular sieve analog.The former powder of the SAPO molecular sieve analog is in Selective Separation/extraction metal ion
Using, be by the former powder of SAPO molecular sieve analog and/or containing the former powder of SAPO molecular sieve analog from
Sub- exchanger is contacted with the liquid-phase system containing metal ion, and metal ion is extracted to solid phase from liquid phase
In.The former powder of the SAPO molecular sieve analog is that can be used for preparing ion-exchanger, can also be straight
Connect and used as ion-exchanger.
Those skilled in the art according to specific requirement, can select the former powder of SAPO molecular sieve analog in choosing
Temperature and time during selecting property separated/extracted metal ion.Preferably, the specific ion exchanger
During separated/extracted, temperature is in the range of 40 DEG C to 90 DEG C, and extraction time is in 0.5h~10h.
Preferably, octatomic ring duct is included in the skeleton structure of the SAPO molecular sieve analog.
Preferably, the SAPO molecular sieve analog, which is selected from, has AEI, CHA, AFX, RHO
At least one of molecular sieve of structure type.
Preferably, the SAPO molecular sieve analog be selected from SAPO-18, SAPO-56,
At least one of SAPO-34, DNL-6 molecular sieve.
Preferably, the metal ion selected from valence state be+1 valency and/or+divalent metal ion at least
It is a kind of.It is further preferred that the metal ion in copper ion, silver ion, cerium ion extremely
Few one kind.
Preferably, at least one in organic amine of the organic formwork agent selected from carbon number no more than 8
Kind.
Preferably, the organic formwork agent is selected from diethylamine (being abbreviated as DEA), triethylamine and (write a Chinese character in simplified form
For TEA), ethylenediamine (being abbreviated as EDA), tetramethylethylenediamine (being abbreviated as TMEDA), N,
N- diisopropyl ethyl amines (being abbreviated as DIEA), tetraethyl oxyammonia (being abbreviated as TEAOH),
Morpholine, N, N, N, N- tetramethyl -1,6- hexamethylene diamines (being abbreviated as TMHD), hexamethylene diamine, di-n-propylamine,
At least one of diisopropylamine.
Preferably, during Selective Separation/extraction copper ion, the former powder choosing of the SAPO molecular sieve analog
At least one of former powder from SAPO-18, SAPO-56, SAPO-34, DNL-6 molecular sieve.
It is further preferred that during Selective Separation/extraction copper ion, the former powder of the SAPO molecular sieve analog
Middle preferred SAPO-18, SAPO-56, SAPO-34, DNL-6 molecular sieve of SAPO molecular sieve analog
At least one of former powder；Organic amine template is selected from two in the former powder of the SAPO molecular sieve analog
Ethamine, triethylamine, ethylenediamine, tetramethylethylenediamine, N, N- diisopropyl ethyl amines, tetraethyl
Oxyammonia, morpholine, N, N, N are N- tetramethyl -1,6- hexamethylene diamines, hexamethylene diamine, di-n-propylamine, two different
At least one of propylamine.
Preferably, during Selective Separation/extraction silver ion, the former powder of the SAPO molecular sieve analog is
The former powder of SAPO-34 molecular sieves and/or the former powder of SAPO-18 molecular sieves.It is further preferred that choosing
During selecting property separated/extracted silver ion, SAPO quasi-molecule in the former powder of the SAPO molecular sieve analog
Sieve is the former powder of SAPO-34 molecular sieves and/or SAPO-18 molecular sieves；The SAPO quasi-molecule
In the former powder of sieve organic amine template be selected from diethylamine, triethylamine, ethylenediamine, tetramethylethylenediamine,
N, N- diisopropyl ethyl amine, tetraethyl oxyammonia, N, N, N, N- tetramethyls -1,6- hexamethylene diamine,
Hexamethylene diamine, di-n-propylamine, at least one of diisopropylamine.
Preferably, during Selective Separation/extraction cerium ion, the former powder of the SAPO molecular sieve analog is
The former powder of SAPO-56 molecular sieves.It is further preferred that during Selective Separation/extraction cerium ion, institute
It is SAPO-56 molecular sieves to state SAPO molecular sieve analog in the former powder of SAPO molecular sieve analog；Institute
State in the former powder of SAPO molecular sieve analog organic amine template be selected from diethylamine, triethylamine, ethylenediamine,
Tetramethylethylenediamine, N, N- diisopropyl ethyl amines, tetraethyl oxyammonia, N, N, N, N- tetramethyls
Base -1,6- hexamethylene diamines, hexamethylene diamine, di-n-propylamine, at least one of diisopropylamine.
The beneficial effect of the application includes but is not limited to：
(1) this application provides the brand-new ion exchange material of a class, with the molecule containing template
The former powder of sieve as ion-exchanger, in mixing salt solution some metals of selective exchange adsorption from
Son, the relative separation of metal salt is realized by the means of phase transfer.
(2) the application opens the frontier using former powder molecular sieve as ion exchange material.Molecule
Sieve material category is abundant, various structures, it is contemplated that by selecting suitable topological structure, port size
And Template Types, ion selectivity and segregation ratio to former powder molecular sieve regulate and control.
Embodiment
The application is described in detail with reference to embodiment, but the application is not limited to these embodiments.
In embodiment, element composition uses PANalytical Axios advanced x-ray fluorescence spectrometries
Instrument (XRF) is measured.
In embodiment, containing template N, the SAPO-18 of N- diisopropyl ethyl amines (is designated as
SAPO-18-DIEA) use【Document 1】Method synthesis.
【Document 1】：J.Phys.Chem.1994,98,10216-10224.
In embodiment, the SAPO-34 (being designated as SAPO-34-DEA) containing diethyl amine template is adopted
With【Document 2】Method synthesis.
【Document 2】：G.Liu et al./Microporous and Mesoporous Materials 111
(2008)143–149。
In embodiment, the SAPO-34 (being designated as SAPO-34-TMEDA) containing TMEDA is used
【Document 3】Method is synthesized.
【Document 3】J.Mater.Chem.A,2013,1,14206–14213.
In embodiment, containing N, N, N, the SAPO-56 of N- tetramethyl -1,6- hexamethylene diamines is used【Document
4】Method is synthesized.
【Document 4】Microporous and Mesoporous Materials,1999,28(1),
125-137。
In embodiment, the DNL-6 containing diethylamine is used【Document 5】Method is synthesized.
【Document 5】Microporous and Mesoporous Materials,2011,144(1-3),
113-119。
Embodiment 1
Prepare Cu (NO3)2、Zn(NO3)2、Co(NO3)2、Ni(NO3)2、AgNO3Mixed solution,
Wherein Cu (NO3)2、Zn(NO3)2、Co(NO3)2、Ni(NO3)2、AgNO3Concentration be
0.01mol/L.According to 1:30 solid-to-liquid ratio, adds 90mL by 3g SAPO-18-DIEA and mixes molten
Liquid, after stirring 3 minutes, is warming up under 50 DEG C, stirring condition and exchanges 4h.It is then centrifuged for separation,
Solid phase is washed with deionized three times, 100 DEG C of drying, Cu, Zn, Co, Ni, Ag in solid phase
Content is determined using XRF.Cu weight/mass percentage compositions therein contain for 0.12%, Zn quality percentage
The weight/mass percentage composition that the weight/mass percentage composition measured as 0.04%, Co is 0.008%, Ni is 0.01%,
Ag weight/mass percentage composition is 0.276%；In solid phase, Cu, Zn, Co, Ni, Ag mol ratio
For Cu：Zn：Co：Ni：Ag=0.19：0.06：0.01：0.02：0.26.
As can be seen that SAPO-18-DIEA can be from containing the molten of copper, zinc, cobalt, nickel and silver ion
In liquid, selective extraction Cu ions and Ag ions.
Embodiment 2
Specific experiment condition and step be the same as Example 1, difference is, by SAPO-18-DIEA
It is substituted for SAPO-34-TMEDA.After exchange, Cu weight/mass percentage compositions are 0.6%, Zn in solid phase
Weight/mass percentage composition be 0.1%, Co weight/mass percentage composition be 0.015%, Ni quality percentage contain
The weight/mass percentage composition measured as 0.017%, Ag is 0.46%；In solid phase, Cu, Zn, Co, Ni,
Ag mol ratio is Cu：Zn：Co：Ni：Ag=0.94：0.15：0.03：0.03：0.43.
As can be seen that SAPO-34-TMEDA can be from containing copper, zinc, cobalt, nickel and silver ion
In solution, selective extraction Cu ions and Ag ions.
Embodiment 3
Specific experiment condition and step be the same as Example 1, difference is, by SAPO-18-DIEA
It is substituted for SAPO-56-TMHD.After exchange, Cu weight/mass percentage compositions are 0.41%, Zn in solid phase
Weight/mass percentage composition be that 0.071%, Co weight/mass percentage composition is 0.009%, Ni quality percentage
The weight/mass percentage composition that content is 0.01%, Ag is 0.107%；In solid phase, Cu, Zn, Co, Ni,
Ag mol ratio is Cu：Zn：Co：Ni：Ag=0.65：0.11：0.02：0.03：0.1.
As can be seen that SAPO-56-TMEDA can be from containing copper, zinc, cobalt, nickel and silver ion
In solution, the extraction Cu ions of high selectivity.
Embodiment 4
Prepare Cu (NO3)2、Zn(NO3)2、Co(NO3)2、Ni(NO3)2Mixed solution, wherein
Cu(NO3)2、Zn(NO3)2、Co(NO3)2、Ni(NO3)2Concentration be 0.05mol/L.According to 1:30
Solid-to-liquid ratio, 3g SAPO-34-TMEDA are entered into 90mL mixed solutions, after stirring 3 minutes,
It is warming up under 50 DEG C, stirring condition and exchanges 4h.Separation is then centrifuged for, solid phase is washed with deionized
Three times, 100 DEG C of drying, Cu in solid phase, Zn, Co, Ni, content using XRF determinations.Its
In Cu weight/mass percentage compositions be that 0.78%, Zn weight/mass percentage composition is 0.08%, Co quality
The weight/mass percentage composition that percentage composition is 0.011%, Ni is 0.014%；In solid phase, Cu, Zn, Co,
Ni mol ratio is Cu：Zn：Co：Ni=1.23：0.12：0.02：0.02.
As can be seen that SAPO-34-TMEDA can be from the solution containing copper, zinc, cobalt and nickel ion
In, the extraction Cu ions of high selectivity.
Embodiment 5
Specific experiment condition and step be the same as Example 4, difference is, by SAPO-34-TMEDA
It is substituted for SAPO-34-DEA.After exchange, Cu weight/mass percentage compositions are 2.13%, Zn in solid phase
Weight/mass percentage composition be that 0.41%, Co weight/mass percentage composition is 0.038%, Ni quality percentage
Content is 0.016%；In solid phase, Cu, Zn, Co, Ni mol ratio are Cu：Zn：Co：Ni=3.35：
0.63：0.06：0.03.
As can be seen that SAPO-34-DEA can from the solution containing copper, zinc, cobalt and nickel ion,
The extraction Cu ions of high selectivity.
Embodiment 6
Prepare AgNO3、Zn(NO3)2、Co(NO3)2、Ni(NO3)2、Mn(NO3)2Mixed solution,
Wherein AgNO3、Zn(NO3)2、Co(NO3)2、Ni(NO3)2、Mn(NO3)2Concentration be
0.01mol/L.According to 1:30 solid-to-liquid ratio, is put into 90mL by 3g SAPO-34-DEA and mixes molten
Liquid, after stirring 3 minutes, is warming up under 50 DEG C, stirring condition and exchanges 4h.Separation is then centrifuged for, Gu
Mutually it is washed with deionized three times, 100 DEG C of drying, Ag, Zn, Co, Ni, Mn in solid phase
Content is determined using XRF.Ag weight/mass percentage compositions therein contain for 3.6%, Zn quality percentage
The weight/mass percentage composition that the weight/mass percentage composition measured as 0.3%, Co is 0.09%, Ni is 0.016%,
Mn percentage composition is 0.02%；In solid phase, Ag, Zn, Co, Ni, Mn mol ratio are Ag：
Zn：Co：Ni：Mn=3.34：0.46：0.15：0.03：0.04.
As can be seen that SAPO-34-DEA can be from containing the molten of silver, zinc, cobalt, nickel and manganese ion
In liquid, the extraction Ag ions of high selectivity.
Embodiment 7
Prepare Ce (NO3)3、Zn(NO3)2、Co(NO3)2、Ni(NO3)2、Mn(NO3)2Mixing it is molten
Liquid, wherein Ce (NO3)3、Zn(NO3)2、Co(NO3)2、Ni(NO3)2、Mn(NO3)2Concentration it is equal
For 0.01mol/L.According to 1:30 solid-to-liquid ratio, contains N, N, N by 3g, N- tetramethyls -1,6- oneself two
The SAPO-56 of amine is put into 90mL mixed solutions, after stirring 3 minutes, is warming up to 50 DEG C, stirring bar
4h is exchanged under part.Separation is then centrifuged for, solid phase is washed with deionized three times, 100 DEG C of drying, Gu
Ce, Zn, Co, Ni, Mn content are determined using XRF in phase.Ce mass percentage therein contains
The weight/mass percentage composition that the weight/mass percentage composition measured as 3.7%, Zn is 0.25%, Co is 0.05%,
The percentage composition that Ni weight/mass percentage composition is 0.01%, Mn is 0.01%；In solid phase, Ce, Zn,
Co, Ni, Mn mol ratio are Ce：Zn：Co：Ni：Mn=2.64：0.38：0.08：0.02：
0.02。
As can be seen that contain N, N, N, the SAPO-56 of N- tetramethyl -1,6- hexamethylene diamines can from containing
In silver, zinc, cobalt, the solution of nickel and manganese ion, the extraction cerium ion of high selectivity.
Embodiment 8
Prepare Cu (NO3)2、Zn(NO3)2、Co(NO3)2、Ni(NO3)2、Mn(NO3)2Mixing it is molten
Liquid, wherein Cu (NO3)2、Zn(NO3)2、Co(NO3)2、Ni(NO3)2、Mn(NO3)2Concentration it is equal
For 0.01mol/L.According to 1:30 solid-to-liquid ratio, 90mL is put into by the 3g DNL-6 for containing diethylamine
Mixed solution, after stirring 3 minutes, is warming up under 50 DEG C, stirring condition and exchanges 4h.It is then centrifuged for point
Be washed with deionized three times from, solid phase, 100 DEG C of drying, Cu in solid phase, Zn, Co, Ni,
Mn content is determined using XRF.Cu weight/mass percentage compositions therein are 2.4%, Zn quality
The weight/mass percentage composition that percentage composition is 0.2%, Co is that 0.14%, Ni weight/mass percentage composition is
0.012%, Mn percentage composition are 0.04%；In solid phase, Cu, Zn, Co, Ni, Mn's rubs
You are than being Cu：Zn：Co：Ni：Mn=3.78：0.31：0.24：0.02：0.07.
As can be seen that the DNL-6 containing diethylamine can be from containing copper, zinc, cobalt and nickel ion
In solution, the extraction Cu ions of high selectivity.
It is described above, only it is several embodiments of the application, any type of limit is not done to the application
System, although the application with preferred embodiment disclose as above, but and be not used to limit the application, it is any
Those skilled in the art, in the range of technical scheme is not departed from, are taken off using above-mentioned
The technology contents shown make a little variation or modification is equal to equivalence enforcement case, belong to technology
In aspects.
Claims (10)
1. application of the former powder of SAPO molecular sieve analog in Selective Separation/extraction metal ion,
Characterized in that, the former powder of the SAPO molecular sieve analog is the SAPO containing organic formwork agent
Molecular sieve analog.
2. application according to claim 1, it is characterised in that the SAPO quasi-molecule
Octatomic ring duct is included in the skeleton structure of sieve.
3. application according to claim 1, it is characterised in that the SAPO quasi-molecule
Screened from least one of molecular sieve with AEI, CHA, AFX, RHO structure type.
4. application according to claim 1, it is characterised in that the SAPO quasi-molecule
Screened from least one of SAPO-18, SAPO-56, SAPO-34, DNL-6 molecular sieve.
5. application according to claim 1, it is characterised in that the metal ion is selected from valency
State is at least one of+1 valency and/or+divalent metal ion；Preferably, the metal ion is selected from
At least one of copper ion, silver ion, cerium ion.
6. application according to claim 1, it is characterised in that the organic formwork agent is selected from
At least one of the organic amine of carbon number no more than 8.
7. application according to claim 1, it is characterised in that the organic formwork agent is selected from
Diethylamine, triethylamine, ethylenediamine, tetramethylethylenediamine, N, N, N, N- tetramethyl -1,6- hexamethylene diamines,
N, N- diisopropyl ethyl amine, hexamethylene diamine, di-n-propylamine, diisopropylamine, tetraethyl oxyammonia,
At least one of morpholine.
8. application according to claim 1, it is characterised in that Selective Separation/extraction copper from
The period of the day from 11 p.m. to 1 a.m, the former powder of the SAPO molecular sieve analog be selected from SAPO-18, SAPO-56, SAPO-34,
At least one of former powder of DNL-6 molecular sieves.
9. application according to claim 1, it is characterised in that Selective Separation/extraction silver from
The period of the day from 11 p.m. to 1 a.m, the former powder of the SAPO molecular sieve analog be SAPO-34 molecular sieves former powder and/or
The former powder of SAPO-18 molecular sieves.
10. application according to claim 1, it is characterised in that Selective Separation/extraction cerium from
The period of the day from 11 p.m. to 1 a.m, the former powder of the SAPO molecular sieve analog is the former powder of SAPO-56 molecular sieves.
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