CN101164688A - Organic/inorganic substance layered composite functional material and preparation method thereof - Google Patents
Organic/inorganic substance layered composite functional material and preparation method thereof Download PDFInfo
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- CN101164688A CN101164688A CNA2007100151675A CN200710015167A CN101164688A CN 101164688 A CN101164688 A CN 101164688A CN A2007100151675 A CNA2007100151675 A CN A2007100151675A CN 200710015167 A CN200710015167 A CN 200710015167A CN 101164688 A CN101164688 A CN 101164688A
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Abstract
The present invention relates to an organic/inorganic lamellar functional new material and its preparation method. Said invention uses anion lamellar material LDH as host, uses anion surfactant as intercalation guest, and utilizes one-step modification process, ion exchange or calcinations restitution process and adopts intercalation assembly method so as to obtain the organic/inorganic composite adsorption material with ultramolecular lamellar structure. Besides, said invention also provides its chemical formula.
Description
One, technical field
The present invention relates to a kind of organic/inorganic substance layered composite functional material and preparation method thereof, belong to field of functional materials.
Two, background technology
The organic pollution that is present in the environment has constituted very big threat to human health and natural environment ecology, and the removal of organic substance all is the emphasis of environmental problem all the time in the environment.It is one of common technology of present environmental pollution improvement that adsorption technology is disposed of sewage, and this technology is used for the adsorbing and removing trace contaminant more in Treatment of Industrial Water, to reach the purpose of deep purifying.The sorbent used selection of absorption method is the key of adsorption technology.But as adsorbent cost and regeneration expense height such as active carbon, humic-acid kind and resinaes, and there is secondary pollution in used adsorbent at present, makes to use to be subjected to certain limitation.
Because hydrotalcite has bigger specific area and pore structure, the adsorbent that can be used for multiple material, its unique memory effect makes its product of roasting can reconstitute hydrotalcite structure in the aqueous solution, treat in the restructuring procedure aqueous solution that adion also can enter into its structure, thereby increased its adsorption capacity, made hydrotalcite and product of roasting thereof become the adsorbent that a kind of utmost point has researching value.If with utilizing again after the burning of the adsorbent behind the adsorption treatment sewage, both realized twice laid, also eliminated secondary pollution.
At document (M.V.Villa, M.J.Sanchez-Martin, M.Sanchez-Camazano, J.Environ.SCi.HealthB34 (1999) 509-525) natural clay class mineral, especially 2: 1 natural cationic clay ore deposit is for cationic and have the organic and inorganic pollutant than high polarity to have adsorption effect preferably.Natural and human synthetic inorganic anion hydrotalcite (LDHs) has the good adsorption effect for the organic and inorganic pollutant of anionic.But for the hydrophobic organic pollutant of nonionic, the adsorption effect of cationic clay and inorganic anion hydrotalcite is all not obvious.
At patent (Duan Xue, Zhang Hui, Wang Bin. a kind of stratiform adsorption functional material at hydrophobic organic and preparation method thereof. Chinese patent: 200410009883.9, the 2005-06-29.) hydrotalcite of anion surfactant modification has removal effect preferably to hydrophobic organic compound.But because modification temperature is low, required modification time is long, and is little to organic adsorbance.
Three, summary of the invention
The object of the present invention is to provide a kind of organic/inorganic substance layered composite functional material and preparation method thereof.Solved natural clay and hydrotalcite adsorbent only to ionic with have the problem that has better adsorption effect than the high polarity organic matter, realized that all kinds of organic pollutions effectively adsorb, thereby reached the purpose of prevention and cure of pollution and environment remediation.
The present invention uses the method for intercalation assembling, sulfonic acid, sulfate anion, the carboxylate radical surfactant that will have long hydrophobic carbochain are assembled into the LDHs interlayer, having prepared a kind of interlayer is the organic/inorganic composite adsorption function material of organic facies, depend on the hydrophobic performance that interlayer distributes phase, hydrophobic organic is produced distribute absorption.This class sorbing material, adsorbs to strengthen by means of hydrophobic interaction stronger between its surface and hydrophobic organic owing to have hydrophobic properties of the surface.
A kind of organic/inorganic substance layered composite functional material of the present invention possesses the stratiform supramolecular structure, and its crystal structure is the crystal structure of houghite material, and its chemical formula is:
(M
2+)
1-x(M
3+)
x(OH)
2(A
-)
a(B
n-)
b·mH
2O；
M wherein
2+Be Zn
2+, Mg
2+, Ca
2+In the divalent ion any one;
M
3+Be Al
3+, Fe
3+, Ga
3+, Ti
3+Deng in the trivalent ion any one;
A
-Be the surfactant anion of interlayer, for carbon number is in 8 ~ 20 alkyl sulfate, alkyl azochlorosulfonate, long-chain carboxylic acid, the aromatic alkyl azochlorosulfonate acid anion any one;
B
N-For carrying capacity is the inorganic anion of n, comprise CO
3 2-, NO
3 -, CI
-, Br
-, I
-, OH
-, H
2PO
4 -In any 1 ~ 3 kind;
0.1＜X＜0.6; A, b are respectively A
-, B
N-Quantity, a+n * b=X; M=0.2-2 is crystallization water quantity.
Wherein, this organic/inorganic substance layered composite functional material crystal structure is the crystal structure of houghite material, is the stratiform supermolecular intercalation structure.
Wherein, this organic/inorganic substance layered composite functional material is applied to adsorb the organic pollution in the environment.
The layered composite functional material its preparation method of this organic/inorganic thing is as follows: a step modification method:
Solubility divalent metal salt and trivalent metal salt are pressed M
2+: M
3+=1 ~ 9: 1 mol ratio is made into total concentration 0.1～3mol/L mixing salt solution A with the deionized water of carbon dioxide removal, with the NaOH solution B of the deionized water of carbon dioxide removal preparation 0.1～1.0mol/L, in addition with the surfactant salt solution C of the deionized water preparation 12 ~ 40mmol/L of carbon dioxide removal;
At N
2Simultaneously slowly be added drop-wise in the container mixing salt solution A and B under the protective condition, the pH of control mixed serum is 7 ~ 13, the sediment D that slurries obtain after suction filtration, washing, D is added in the autoclave, the surfactant salt solution C that adds 5 times of quality of sediment simultaneously, mixed liquor at 100 ~ 160 ℃ of following crystallization 30min, again through suction filtration, washing and drying, is obtained surfactant intercalated hydrotalcite;
Perhaps ion-exchange:
The sediment D that obtains after suction filtration, the washing in the one step modification method was worn out 6 hours down at 60-150 ℃, obtain inorganic anion hydrotalcite (M
2+)
1-x(M
3+)
x(OH)
2(A
-)
a(B
N-)
bMH
2O must mix with the surfactant salt solution C of its 5 times of quality and be added in the autoclave obtaining the inorganic anion hydrotalcite, makes mixed liquor react 30min down at 100 ~ 160 ℃, again through suction filtration, washing and drying, obtains surfactant intercalated hydrotalcite;
Perhaps roasting is restored:
Inorganic anion hydrotalcite (the M that ion-exchange is obtained
2+)
1-x(M
3+)
x(OH)
2(A
-)
a(B
N-)
bMH
2O was 400～500 ℃ of following roastings 1 hour, obtain mixing bimetallic oxide (LDO), LDO mixed with the surfactant salt solution C of its 5 times of quality and change and add in the autoclave, make mixed liquor react 30min down at 100 ~ 160 ℃, through suction filtration, washing and drying, obtain surfactant intercalated hydrotalcite again;
Wherein: above-mentioned M
2+Be Zn
2+, Mg
2+, Ca
2+In any; M
3+Be Al
3+, Fe
3+, Ga
3+, Ti
3+In any; A
-Be the surfactant anion of interlayer, for carbon number is in 8 ~ 20 alkyl sulfate, alkyl azochlorosulfonate, long-chain carboxylic acid, the aromatic alkyl azochlorosulfonate acid anion any one; B
N-For carrying capacity is the inorganic anion of n, be CO
3 2-, NO
3 -, Cl
-In any; 0.1＜X＜0.6; A, b are respectively A
-, B
N-Quantity, g+n * b=X; M=0.2-2 is crystallization water quantity.
The surfactant intercalated hydrotalcite that obtains is implemented X-ray powder diffraction characterize, characterization result is shown in Figure 1.Display surface activating agent anion has inserted hydrotalcite layers as a result, and surfactant intercalated hydrotalcite has the layer dress supramolecular structure of hydrotalcite-like material.
Surfactant intercalated hydrotalcite has regular layer structure, has main body laminate and interlayer object surfactant anion that the metal oxygen atom is constituted, and the two interacts in conjunction with forming a kind of structure closely by covalent bond and hydrogen bond etc.; The orderly gathering of surfactant makes interlayer form a hydrophobic region, and the existence of this hydrophobic distribution phase makes this material produce distribution absorption to the hydrophobic organic in the water.
Surfactant intercalated hydrotalcite is to the static adsorption test 1 of hydrophobic organic para-nitrotoluene:
Prepare the para-nitrotoluene solution of a series of concentration, lauryl sodium sulfate intercalation magnalium hydrotalcite (MHT-1) sample mix of respectively getting above-mentioned solution of 50ml and 50mg places the tool plug triangular flask of 100ml, be placed in the oscillator, continuous oscillation under 140 times/minute the vibration velocity more than 4 hours to guarantee to reach adsorption equilibrium, measure concentration C before (day island proper Tianjin UV-2550) absorption with ultraviolet specrophotometer respectively
0And the concentration C e after the adsorption equilibrium.According to formula Q
e=(C
0-Ce) * and V/W calculates equilibrium adsorption capacity, and hydrotalcite was to the adsorbance of para-nitrotoluene, C when Qe was balance in the formula
0Be the initial concentration (mg/L) of solution, the concentration of para-nitrotoluene (mg/L) in liquid phase when Ce is balance, V is the volume (L) of para-nitrotoluene solution in the absorption system, W is the quality (g) of adsorbent in the absorption system, with Qe to C
0Mapping promptly gets the static balancing adsorption isotherm of MHT-1 to para-nitrotoluene, is plotted in Fig. 2.
Surfactant intercalated hydrotalcite is to the static adsorption test 2 of hydrophobic organic para-nitrotoluene:
Prepare the para-nitrotoluene solution of a series of concentration, the MHT-3 sample mix of respectively getting above-mentioned solution of 50ml and 50mg places the tool plug triangular flask of 50ml, be placed in the oscillator, continuous oscillation under 140 times/minute the vibration velocity more than 4 hours to guarantee to reach adsorption equilibrium, measure concentration C before (day island proper Tianjin UV-2550) absorption with ultraviolet specrophotometer respectively
0And the concentration C e after the adsorption equilibrium.According to formula Q
e=(C
0-Ce) * and V/W calculates equilibrium adsorption capacity, and hydrotalcite was to the adsorbance of para-nitrotoluene, C when Qe was balance in the formula
0Be the initial concentration (mg/L) of solution, the concentration of para-nitrotoluene (mg/L) in liquid phase when Ce is balance, V is the volume (L) of para-nitrotoluene solution in the absorption system, W is the quality (g) of adsorbent in the absorption system, with Qe to C
0Mapping promptly gets the static balancing adsorption isotherm of MHT-3 to para-nitrotoluene, is plotted in Fig. 2.
Advantage of the present invention is: the complex layered functional material method of stratiform organic/inorganic that preparation has the organic matter adsorption function is simple, modification time is short, adsorbance is big, and can select corresponding preparation method for use according to different conditions and demand, the supermolecular intercalation assemble method is used to prepare surfactant intercalated hydrotalcite, be applied to adsorb machine thing in the environment, the space of the controlled design of material is bigger, can be at different organic matters, and different demands carries out the design of sorbent structure and the modulation of chemical composition, as the kind and the element ratio of laminate element, the kind of interlayer surface active anion and quantity etc. can be achieved by the synthesis condition of adjusting adsorbent.
Four, description of drawings
Fig. 1 is the X-ray powder diffraction figure of lauryl sodium sulfate intercalated houghite under the embodiment of the invention 1-3 assembling condition.Wherein abscissa is an angle of diffraction, and ordinate is a diffraction peak intensity.
Fig. 2 is the static adsorption isotherm of the hydrophobic para-nitrotoluene of the lauryl sodium sulfate intercalation magnalium hydrotalcite absorption of embodiment of the invention 1-3 preparation.Wherein abscissa is the absorption initial concentration, and ordinate is an adsorbance.
Five, the specific embodiment
Mg (NO with 30.8g
3)
26H
2Al (the NO of O and 15g
3)
39H
2O is made into the mixing salt solution A that the Mg/Al mol ratio equals 3 with 400ml water; With taking off CO
2The deionized water compound concentration be the NaOH solution B of 0.48mol/L; With taking off CO
2The deionized water compound concentration is lauryl sodium sulfate (SDS) solution C of 12mmol/L;
At N
2Under the protective condition mixing salt solution A and B slowly are added drop-wise in the container simultaneously, the pH of control slurries is 9 ~ 12;
The gained slurries are transferred to behind suction filtration in the autoclave, add 50ml surfactant salt solution C simultaneously, make mixed liquor at 100～160 ℃ of following crystallization 30min, again through suction filtration, washing and drying, obtain surfactant intercalated hydrotalcite (MHT-1).
The MHT-1 that obtains is carried out X-ray powder diffraction characterize, the results are shown in Figure 1, MHT-1 has the crystal structure of hydrotalcite-like material as seen from Figure 1, and the characteristic diffraction peak of SDS is arranged, and illustrates that the dodecyl sulphate anion is between insert layer.
Mg (NO with 30.8g
3)
26H
2Al (the NO of O and 15g
3)
39H
2O is made into the mixing salt solution A that the Mg/Al mol ratio equals 3 with 400ml water; With taking off CO
2The deionized water compound concentration be the NaOH solution B of 0.48mol; With taking off CO
2The deionized water compound concentration is the sodium dodecyl sulfate solution C of 12mmol/L;
At N
2Under the protective condition mixing salt solution A and B slowly are added drop-wise in the container simultaneously, the pH of control slurries is 9 ~ 12; With gained slurries suction filtration, washing obtains the sediment filter cake, and filter cake is transferred in the wide-mouth bottle, obtains nitrate anion type inorganic anion hydrotalcite sample behind 80 ℃ of water-bath 6h.
Hydrotalcite is mixed with 50ml surfactant salt solution C and be transferred in the autoclave, make mixed liquor,, obtain surfactant intercalated hydrotalcite (MHT-2) again through suction filtration, washing and drying at 100～160 ℃ of reaction 30min down;
The MHT-2 that obtains is carried out X-ray powder diffraction to be characterized, the results are shown in Figure 1, nitrate anion type inorganic anion hydrotalcite sample (HT) well-crystallized as seen from Figure 1, MHT-2 after the SDS modification has the crystal structure of hydrotalcite-like material, and the characteristic diffraction peak that SDS is arranged illustrates that the dodecyl sulphate anion is between insert layer.
Mg (NO with 30.8g
3)
26H
2Al (the NO of O and 15g
3)
39H
2O is made into the mixing salt solution A that the Mg/Al mol ratio equals 3 with 400ml water; With taking off CO
2The deionized water compound concentration be the NaOH solution B of 0.48mol; With taking off CO
2The deionized water compound concentration is the sodium dodecyl sulfate solution C of 12mmol/L;
At N
2Under the protective condition mixing salt solution A and B slowly are added drop-wise in the container simultaneously, the pH of control slurries is 8 ~ 13; With gained slurries suction filtration, washing obtains the sediment filter cake, and filter cake is transferred in the wide-mouth bottle, obtains nitrate anion type inorganic anion hydrotalcite sample behind 80 ℃ of water-bath 6h.
With this nitrate anion type inorganic anion hydrotalcite sample 400～500 ℃ of roastings, obtain bimetallic oxide LDO, LDO is mixed with 50ml surfactant salt solution C and be transferred in the autoclave, make mixed liquor react 30min down at 100～160 ℃, through suction filtration, washing and drying, obtain surfactant intercalated hydrotalcite (MHT-3) again.
Claims (4)
1. organic/inorganic substance layered composite functional material, chemical formula is:
(M
2+)
1-x(M
3+)
x(OH)
2(A
-)
a(B
n-)
b·mH
2O；
M wherein
2+Be Zn
2+, Mg
2+, Ca
2+In the divalent ion any one;
M
3+Be Al
3+, Fe
3+, Ga
3+, Ti
3+Deng in the trivalent ion any one;
A
-Be the surfactant anion of interlayer, for carbon number is in 8 ~ 20 alkyl sulfate, alkyl azochlorosulfonate, long-chain carboxylic acid, the aromatic alkyl azochlorosulfonate acid anion any one;
B
N-For carrying capacity is the inorganic anion of n, comprise CO
3 2-, NO
3 -, CI
-, Br
-, I
-, OH
-, H
2PO
4 -In any 1 ~ 3 kind;
0.1＜X＜0.6; A, b are respectively A
-, B
N-Quantity, a+n * b=X; M=0.2-2 is crystallization water quantity.
2. a kind of organic/inorganic substance layered composite functional material as claimed in claim 1 is characterized in that: its structure is the crystal structure of houghite material, is the stratiform supermolecular intercalation structure.
3. a kind of organic/inorganic substance layered composite functional material as claimed in claim 1 or 2, it is characterized in that: this adsorption functional material is applied to adsorb the organic pollution in the environment.
4. the preparation method of the layered composite functional material of the described a kind of organic/inorganic thing of claim 1, step is as follows: a step modification method:
Solubility divalent metal salt and trivalent metal salt are pressed M
2+: M
3+=1 ~ 9: 1 mol ratio is made into total concentration 0.1～3mol/L mixing salt solution A with the deionized water of carbon dioxide removal, with the NaOH solution B of the deionized water of carbon dioxide removal preparation 0.1～1.0mol/L, in addition with the surfactant salt solution C of the deionized water preparation 12 ~ 40mmol/L of carbon dioxide removal;
At N
2Simultaneously slowly be added drop-wise in the container mixing salt solution A and B under the protective condition, the pH of control mixed serum is 7 ~ 13, the sediment D that slurries obtain after suction filtration, washing, D is added in the autoclave, the surfactant salt solution C that adds 5 times of quality of sediment simultaneously, mixed liquor at 100 ~ 160 ℃ of following crystallization 30min, again through suction filtration, washing and drying, is obtained surfactant intercalated hydrotalcite;
Perhaps ion-exchange:
The sediment D that obtains after suction filtration, the washing in the one step modification method was worn out 6 hours down at 60-150 ℃, obtain inorganic anion hydrotalcite (M
2+)
1-x(M
3+)
x(OH)
2(A
-)
a(B
N-)
bMH
2O must mix with the surfactant salt solution C of its 5 times of quality and be added in the autoclave obtaining the inorganic anion hydrotalcite, makes mixed liquor react 30min down at 100 ~ 160 ℃, again through suction filtration, washing and drying, obtains surfactant intercalated hydrotalcite;
Perhaps roasting is restored:
Inorganic anion hydrotalcite (the M that ion-exchange is obtained
2+)
1-x(M
3+)
x(OH)
2(A
-)
a(B
N-)
bMH
2O was 400～500 ℃ of following roastings 1 hour, obtain mixing bimetallic oxide (LDO), LDO mixed with the surfactant salt solution C of its 5 times of quality and change and add in the autoclave, make mixed liquor react 30min down at 100 ~ 160 ℃, through suction filtration, washing and drying, obtain surfactant intercalated hydrotalcite again;
Wherein: above-mentioned M
2+Be Zn
2+, Mg
2+, Ca
2+In any; M
3+Be Al
3+, Fe
3+, Ga
3+, Ti
3+In any; A
-Be the surfactant anion of interlayer, for carbon number is in 8 ~ 20 alkyl sulfate, alkyl azochlorosulfonate, long-chain carboxylic acid, the aromatic alkyl azochlorosulfonate acid anion any one; B
N-For carrying capacity is the inorganic anion of n, be CO
3 2-, NO
3 -, Cl
-In any; 0.1＜X＜0.6; A, b are respectively A
-, B
N-Quantity, a+n * b=X; M=0.2-2 is crystallization water quantity.
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| CN102335627A (en) * | 2011-06-28 | 2012-02-01 | 太原理工大学 | Preparation method of metal complex functionalized hydrotalcite-like nano-layer sheet |
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| CN102335627B (en) * | 2011-06-28 | 2013-03-06 | 太原理工大学 | Preparation method of metal complex functionalized hydrotalcite-like nano-layer sheet |
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| CN106881067A (en) * | 2017-04-24 | 2017-06-23 | 北京化工大学 | A kind of modified houghite adsorbent and its application |
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| Qiu et al. | Removal of lead, copper, nickel, cobalt, and zinc from water by a cancrinite-type zeolite synthesized from fly ash | |
| Cheng et al. | Phosphate adsorption from sewage sludge filtrate using zinc–aluminum layered double hydroxides | |
| Xiao et al. | The influence of ferric iron in calcined nano-Mg/Al hydrotalcite on adsorption of Cr (VI) from aqueous solution | |
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| Abo-El-Enein et al. | Removal of some heavy metals ions from wastewater by copolymer of iron and aluminum impregnated with active silica derived from rice husk ash | |
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