CN102502672A - Layered multi-stage zinc silicate and preparation method and application thereof - Google Patents
Layered multi-stage zinc silicate and preparation method and application thereof Download PDFInfo
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- CN102502672A CN102502672A CN2011103289202A CN201110328920A CN102502672A CN 102502672 A CN102502672 A CN 102502672A CN 2011103289202 A CN2011103289202 A CN 2011103289202A CN 201110328920 A CN201110328920 A CN 201110328920A CN 102502672 A CN102502672 A CN 102502672A
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- 239000004110 Zinc silicate Substances 0.000 title claims abstract description 46
- XSMMCTCMFDWXIX-UHFFFAOYSA-N zinc silicate Chemical compound [Zn+2].[O-][Si]([O-])=O XSMMCTCMFDWXIX-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 235000019352 zinc silicate Nutrition 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 32
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 20
- 239000010703 silicon Substances 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 16
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 15
- 150000003751 zinc Chemical class 0.000 claims abstract description 13
- 150000003863 ammonium salts Chemical class 0.000 claims abstract description 11
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 7
- 150000002500 ions Chemical class 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 5
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 12
- RVPVRDXYQKGNMQ-UHFFFAOYSA-N lead(2+) Chemical compound [Pb+2] RVPVRDXYQKGNMQ-UHFFFAOYSA-N 0.000 claims description 12
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 10
- 235000019353 potassium silicate Nutrition 0.000 claims description 9
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 8
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 7
- 235000019270 ammonium chloride Nutrition 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 229910001385 heavy metal Inorganic materials 0.000 claims description 5
- 239000011592 zinc chloride Substances 0.000 claims description 5
- 235000005074 zinc chloride Nutrition 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 4
- LDDQLRUQCUTJBB-UHFFFAOYSA-N ammonium fluoride Chemical compound [NH4+].[F-] LDDQLRUQCUTJBB-UHFFFAOYSA-N 0.000 claims description 4
- 239000004246 zinc acetate Substances 0.000 claims description 4
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims description 2
- 239000004111 Potassium silicate Substances 0.000 claims description 2
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 claims description 2
- NNHHDJVEYQHLHG-UHFFFAOYSA-N potassium silicate Chemical compound [K+].[K+].[O-][Si]([O-])=O NNHHDJVEYQHLHG-UHFFFAOYSA-N 0.000 claims description 2
- 229910052913 potassium silicate Inorganic materials 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 2
- 229960001763 zinc sulfate Drugs 0.000 claims description 2
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims 1
- 235000012239 silicon dioxide Nutrition 0.000 claims 1
- 229960001866 silicon dioxide Drugs 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 11
- 238000001179 sorption measurement Methods 0.000 abstract description 10
- 230000000694 effects Effects 0.000 abstract description 5
- 239000004113 Sepiolite Substances 0.000 abstract description 3
- 229910052624 sepiolite Inorganic materials 0.000 abstract description 3
- 235000019355 sepiolite Nutrition 0.000 abstract description 3
- 229910052604 silicate mineral Inorganic materials 0.000 abstract description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract 1
- 238000000746 purification Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 20
- 239000008367 deionised water Substances 0.000 description 10
- 229910021641 deionized water Inorganic materials 0.000 description 10
- 238000000634 powder X-ray diffraction Methods 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- 238000011068 loading method Methods 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
- 239000012467 final product Substances 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 239000002086 nanomaterial Substances 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 230000000274 adsorptive effect Effects 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 238000012512 characterization method Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- -1 plumbum ion Chemical class 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000000371 solid-state nuclear magnetic resonance spectroscopy Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000001132 ultrasonic dispersion Methods 0.000 description 2
- 241000446313 Lamella Species 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000112 cooling gas Substances 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 238000000295 emission spectrum Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 244000144992 flock Species 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- DNHVXYDGZKWYNU-UHFFFAOYSA-N lead;hydrate Chemical compound O.[Pb] DNHVXYDGZKWYNU-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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- Silicates, Zeolites, And Molecular Sieves (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Water Treatment By Sorption (AREA)
Abstract
The invention discloses layered multi-stage zinc silicate and a preparation method and application thereof. The method comprises the following step of: preparing the layered multi-stage zinc silicate from a silicon source and soluble zinc salt serving as raw materials by a one-step hydrothermal method under the combined action of inorganic ammonium salt and ammonia water. The layered multi-stage zinc silicate nanometer material has the large specific surface area (200 to 300m<2>/g) and a unique wide-gap layered structure (the layer gap is about 1.22nm), is used for adsorbing lead ions in water, and has an obvious effect, high adsorption capacity (201 to 210mg/g), and purification capacity which is obviously higher than that of the currently used natural silicate mineral, namely sepiolite.
Description
Technical field
The present invention relates to multistage zinc silicate of a kind of stratiform and preparation method thereof and application.
Background technology
Micro-nano multilevel hierarchy material because of it possesses the good mechanical property of high-ratio surface, high reactivity and the micro-meter scale of nanoscale simultaneously, is easy to advantages such as actually operating, has wide application prospect in fields such as catalysis, absorption.Usually the hierarchy of report, flower-like structure for example, the essentially consist unit of its petal is a nano particle.The multistage zinc silicate material that the present invention relates to, its petal are unique laminate structure.This laminate structure is beneficial to the transmission of material on the one hand because of its bigger interlamellar spacing, it has the potential using value in absorption, host-guest chemistry; The confinement effect of interlayer can be used for preparing other nano material on the other hand.Do not see the structure report of the multistage zinc silicate of this kind stratiform at present in the document as yet.
Silicate material is one type of inorganic adsorbent that is utilized by broad research.For example, the decolouring in the sugar industry is handled, and has just adopted a kind of natural silicate mineral, sepiolite.And a main application of multilevel hierarchy material is exactly as sorbing material.In conjunction with the silicate multilevel hierarchy material of both advantages, in water treatment, show excellent adsorptive power, particularly heavy metal ion.In the considerable area of China, contain excessive lead ion in the underground water, have a strong impact on people's life and health.The specified concentration of the Pb in Drinking Water of The World Health Organization's regulation is 10 μ g/L.Further the efficient water treatment absorbent of development of new has great practical significance.
Summary of the invention
The purpose of this invention is to provide a kind of multistage zinc silicate of stratiform of removing heavy-metal pollution thing in the water and preparation method thereof that can be used for adsorbing.
The multistage zinc silicate of stratiform provided by the present invention is to prepare according to the method that comprises the steps: with soluble zinc salt and multiple silicon source is raw material, under the acting in conjunction of inorganic ammonium salt and ammoniacal liquor, makes through one step hydro thermal method.
Concrete preparation method is following:
1) with soluble zinc salt, inorganic ammonium salt and ammonia solvent in water, obtain solution A; Other looks the different dissolvings of silicon source category or ultra-sonic dispersion in water, obtains solution B;
2) said solution A and solution B are mixed, obtain mixed system C (look silicon source category difference and possibly form mixing solutions or flocks);
3) said mixed system C is transferred to carries out hydro-thermal reaction in the closed reactor, obtain layered multistage zinc silicate.
The temperature of reaction of said hydro-thermal reaction is 120-160 ℃, preferred 140-160 ℃; Reaction times is 9-24 hour, preferred 12-24 hour.
In the aforesaid method, the zinc salt of said solubility is generally cheap zinc salt, like zinc chloride, zinc nitrate, zinc acetate or zinc sulfate.
Said silicon source can be water glass, potassium silicate, silicon dioxide powder etc.
Said inorganic ammonium salt can be ammonium chloride, Neutral ammonium fluoride, brometo de amonio or an ammonium nitrate etc.
In the aforesaid method, the mol ratio in said zinc salt and silicon source is 3: (4.5-5.5).The consumption of said inorganic ammonium salt is 8-12mmol.The consumption of said ammoniacal liquor is 0.8-1.2ml.The mol ratio in the consumption of said ammoniacal liquor and silicon source is (5.5-5.6): 1.The mol ratio of said inorganic ammonium salt and ammoniacal liquor is (9.5-10.5): 7.
The multistage zinc silicate nano material of stratiform of the present invention's preparation can be used for the heavy metal ion in the planar water; Especially remarkable to the adsorption effect of lead ion.
Excellent effect of the present invention; The one, adopting the cheap zinc salt and the multiple silicon source of solubility is raw material; Under identical test conditions, all can prepare the multistage zinc silicate nano material of stratiform, this makes that the choice of raw material is very big, and actually operating is flexible and changeable; And method is simple, safety, cost are low, is easy to suitability for industrialized production; The 2nd, the multistage zinc silicate nano material of stratiform of preparation has big specific surface area (200-300m
2/ g) with unique broad gap laminate structure (the about 1.22nm of interlamellar spacing), be used for the planar water lead ion, effect is remarkable, the loading capacity height (～210mg/g), detergent power significantly is better than present employed natural silicate mineral, sepiolite.
Description of drawings
Fig. 1 is the multistage zinc silicate X-ray powder diffraction of embodiment 1 obtained stratiform figure.
Fig. 2 is that the multistage zinc silicate SEM of embodiment 1 obtained stratiform Electronic Speculum detects figure.
Fig. 3 is that the multistage zinc silicate TEM of embodiment 1 obtained stratiform Electronic Speculum detects figure.
Fig. 4 is that the multistage zinc silicate HRTEM of embodiment 1 obtained stratiform Electronic Speculum detects figure.
Fig. 5 is the multistage zinc silicate solid state nmr of embodiment 1 an obtained stratiform silicon spectrum.
Fig. 6 is the multistage zinc silicate nitrogen adsorption of embodiment 1 obtained stratiform-desorption graphic representation.
Fig. 7 is the multistage zinc silicate adsorption isothermal curve of embodiment 1 obtained stratiform figure.
Fig. 8 is the multistage zinc silicate X-ray powder diffraction of embodiment 2 obtained stratiforms figure.
Fig. 9 is that the multistage zinc silicate SEM of embodiment 2 obtained stratiforms Electronic Speculum detects figure.
Figure 10 is the multistage zinc silicate X-ray powder diffraction of embodiment 3 obtained stratiforms figure.
Figure 11 is that the multistage zinc silicate SEM of embodiment 3 obtained stratiforms Electronic Speculum detects figure.
Figure 12 is the multistage zinc silicate X-ray powder diffraction of embodiment 4 obtained stratiforms figure.
Figure 13 is that the multistage zinc silicate SEM of embodiment 4 obtained stratiforms Electronic Speculum detects figure.
Figure 14 is the multistage zinc silicate X-ray powder diffraction of embodiment 5 obtained stratiforms figure.
Figure 15 is that the multistage zinc silicate SEM of embodiment 5 obtained stratiforms Electronic Speculum detects figure.
Embodiment
Through specific embodiment method of the present invention is described below, but the present invention is not limited thereto.
Experimental technique described in the following embodiment like no specified otherwise, is ordinary method; Said reagent and material like no specified otherwise, all can obtain from commercial sources.Used ammoniacal liquor is commercially available ammoniacal liquor among the following embodiment, and its mass concentration is 28%.
Among the following embodiment, adopt JEOL-6701F type sem (SEM), JEOL JEM-1011 type transmission electron microscope (TEM) to characterize pattern; JEM 2100F type high resolution transmission electron microscope (HRTEM) characterizes its laminate structure; Rigaku D/max-2500 type x-ray powder diffraction instrument characterizes its crystalline structure; Adopt Bruker III 400 types to characterize the coordination situation of silicon; Adopt Quantachrome Autosorb-1 type specific surface area and pore distribution analyser to characterize its pore structure.Adopt inductively coupled plasma-atomic emission spectrum (ICP-AES) to detect the concentration of lead ion in the water; Adopt day island proper Tianjin ICPE-9000 plasma emission spectrometer; Test condition is: high frequency output rating 1.20KW, cooling gas flow 0.6L/min, plasma gas flow rate 10L/min; Carrier gas flux 0.7L/min, 30 seconds time shutter.
Embodiment 1: the preparation multistage zinc silicate of stratiform (the silicon source is a water glass)
Cheap zinc chloride (0.75mmol), the ammonium chloride (10mmol) of solubility are scattered in the 30ml deionized water, as solution A with ammoniacal liquor (1ml) dissolving; Water glass (1.266mmol) dissolving is scattered in the 20ml deionized water, as solution B.After the two mixes, be transferred in the 70ml water heating kettle, left standstill 12 hours in 140 degree.After treating naturally cooling, with water washing several times, oven dry gets final product.
Product is accredited as zinc silicate (as shown in Figure 1) through x-ray powder diffraction instrument; With SEM (as shown in Figure 2) and TEM (as shown in Figure 3) its pattern is characterized, can find out that it is the flower-like structure that is assembled by the sheet structure of twisting, size is about 600nm.Further HRTEM characterizes (as shown in Figure 4), can clearly be seen that, the petal of its distortion is novel laminate structure, through measuring interlamellar spacing about 1.22nm.And XRD is at obvious diffraction peak, the 7.2 degree left and right sides, calculates through Bragg equation, the just corresponding numerical value of 1.22nm.The data presentation (as shown in Figure 5) of solid state nmr silicon spectrum; What the chemical shift of-96.9ppm was just corresponding is the silicon of three-fold coordination; Be that silicon is to arrange with the form of hexagonal mesh to form the silicon-oxy tetrahedron lamella, then form the layered silicate of " sandwich " structure of 2: 1 with zinc.It is carried out pore structure characterize (as shown in Figure 6), specific surface area reaches 236m
2/ g, pore volume reaches 0.7cc/g.
This sample is carried out the adsorption test of lead ion in the aqueous solution, and its loading capacity can reach 210mg/g as a result.(as shown in Figure 7).
Embodiment 2: the preparation multistage zinc silicate of stratiform (the silicon source is a silicon dioxide powder)
Cheap zinc chloride (0.75mmol), the ammonium chloride (10mmol) of solubility are scattered in the 30ml deionized water, as solution A with ammoniacal liquor (1ml) dissolving; Silicon dioxide powder (1.266mmol) ultra-sonic dispersion is in the 20ml deionized water, as solution B.After the two mixes, be transferred in the 70ml water heating kettle, left standstill 24 hours in 160 degree.After treating naturally cooling, with water washing several times, oven dry gets final product.X-ray powder diffraction spectrogram and embodiment 1 identical (as shown in Figure 8), the diffraction peak between the 5-10 degree still can be judged its laminate structure; With SEM (as shown in Figure 9) its pattern is characterized, can find out that it also is the flower-like structure that is assembled by the sheet structure of twisting, size is about 600nm.The specific surface area of the multistage zinc silicate of gained stratiform reaches 210m
2/ g.
This sample is carried out the adsorption test of lead ion in the aqueous solution, and its loading capacity can reach 201mg/g as a result.
Embodiment 3: the preparation multistage zinc silicate of stratiform (inorganic ammonium salt is a Neutral ammonium fluoride)
Cheap zinc chloride (0.75mmol), the Neutral ammonium fluoride (10mmol) of solubility are scattered in the 30ml deionized water, as solution A with ammoniacal liquor (1ml) dissolving; Water glass (1.266mmol) dissolving is scattered in the 20ml deionized water, as solution B.After the two mixes, be transferred in the 70ml water heating kettle, left standstill 12 hours in 140 degree.After treating naturally cooling, with water washing several times, oven dry gets final product.Characterization result is identical with embodiment 2.The specific surface area of the multistage zinc silicate of gained stratiform reaches 230m
2/ g.
This sample is carried out the adsorption test of lead ion in the aqueous solution, and its loading capacity can reach 206mg/g as a result.
Embodiment 4: the preparation multistage zinc silicate of stratiform (zinc salt is a zinc nitrate)
Cheap zinc nitrate (0.75mmol), the ammonium chloride (10mmol) of solubility are scattered in the 30ml deionized water, as solution A with ammoniacal liquor (1ml) dissolving; Water glass (1.266mmol) dissolving is scattered in the 20ml deionized water, as solution B.After the two mixes, be transferred in the 70ml water heating kettle, left standstill 12 hours in 140 degree.After treating naturally cooling, with water washing several times, oven dry gets final product.Characterization result is identical with embodiment 2.The specific surface area of the multistage zinc silicate of gained stratiform reaches 232m
2/ g.
This sample is carried out the adsorption test of lead ion in the aqueous solution, and its loading capacity can reach 208mg/g as a result.
Embodiment 5: the preparation multistage zinc silicate of stratiform (zinc salt is a zinc acetate)
Cheap zinc acetate (0.75mmol), the ammonium chloride (10mmol) of solubility are scattered in the 30ml deionized water, as solution A with ammoniacal liquor (1ml) dissolving; Water glass (1.266mmol) dissolving is scattered in the 20ml deionized water, as solution B.After the two mixes, be transferred in the 70ml water heating kettle, left standstill 12 hours in 140 degree.After treating naturally cooling, with water washing several times, oven dry gets final product.Characterization result is identical with embodiment 2.
The specific surface area of the multistage zinc silicate of gained stratiform reaches 225m
2/ g.
This sample is carried out the adsorption test of lead ion in the aqueous solution, and its loading capacity can reach 205mg/g as a result.
Embodiment 6: to the adsorptive power test of lead
With product shown in Figure 1 is a with 10mg; Mix mutually with the lead ion solution 20ml of different concns respectively, afterwards to every part of solution stirring at room after 12 hours, every part of mixed solution spinning; Its upper solution is used the analysis of inductively coupled plasma-Atomic Emission SpectrometerAES respectively; Obtain adsorbing the plumbum ion concentration when reaching balance, combines calculating, obtain the adsorptive capacity of this material lead ion in the corresponding solution with the plumbum ion concentration in the solution before the absorption.At last, obtain the adsorption isothermal curve of this material, see Fig. 7 lead ion according to these data.
Claims (10)
1. a method for preparing the multistage zinc silicate of stratiform comprises the steps: that with silicon source and soluble zinc salt be raw material, under the acting in conjunction of inorganic ammonium salt and ammoniacal liquor, prepares layered multistage zinc silicate through one step hydro thermal method.
2. method according to claim 1 is characterized in that: said silicon source is selected from following at least a: water glass, potassium silicate and silicon-dioxide.
3. method according to claim 1 is characterized in that: said soluble zinc salt is selected from following at least a: zinc chloride, zinc nitrate, zinc acetate and zinc sulfate.
4. method according to claim 1 is characterized in that: said inorganic ammonium salt is selected from following at least a: ammonium chloride, Neutral ammonium fluoride, brometo de amonio and an ammonium nitrate.
5. according to each described method among the claim 1-4, it is characterized in that: the mol ratio in said soluble zinc salt and silicon source is 3: (4.5-5.5); The mol ratio in said ammoniacal liquor and silicon source is (5.5-5.6): 1; The mol ratio of said inorganic ammonium salt and ammoniacal liquor is (9.5-10.5): 7.
6. according to each described method among the claim 1-5, it is characterized in that: the step of said method is following: 1) with soluble zinc salt, inorganic ammonium salt and ammonia solvent in water, obtain solution A; The silicon source is dissolved or dispersed in the water, obtains solution B;
2) said solution A and solution B are mixed, obtain mixed system C;
3) place closed reactor to carry out hydro-thermal reaction said mixed system C, obtain layered multistage zinc silicate.
7. method according to claim 6 is characterized in that: the temperature of reaction of said hydro-thermal reaction is under 120-160 ℃, and the reaction times is 9-24 hour.
8. the multistage zinc silicate of stratiform that each said method prepares among the claim 1-7.
9. the multistage zinc silicate of stratiform according to claim 8 is characterized in that: the specific surface area of layered multistage zinc silicate is 200-300m
2/ g.
10. claim 8 or the application of the multistage zinc silicate of 9 described stratiforms in absorbing heavy metal ions in water; The preferred lead ion of said heavy metal ion.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102976344A (en) * | 2012-12-29 | 2013-03-20 | 石家庄学院 | Preparation method of zinc silicate nanometer material |
| CN104087289A (en) * | 2014-06-30 | 2014-10-08 | 中国石油大学(华东) | Method of synthesizing nano zinc silicate light emitting material by using waste silicon powder by hydrothermal method |
| CN108428882A (en) * | 2018-04-17 | 2018-08-21 | 洛阳理工学院 | A kind of zinc silicate/carbon micro-nano hierarchical structure compound and preparation method thereof |
| CN109824055A (en) * | 2019-04-04 | 2019-05-31 | 河北工业大学 | The method for preparing nano-sheet zinc silicate compound adsorbent using iron tailings |
| CN112221503A (en) * | 2020-10-15 | 2021-01-15 | 山东科技大学 | Multi-level nano array phyllosilicate catalyst and preparation method thereof |
| CN117003253A (en) * | 2023-07-26 | 2023-11-07 | 上海师范大学 | Zinc silicate flower-shaped porous microsphere and preparation method thereof |
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| US4681749A (en) * | 1984-06-22 | 1987-07-21 | Mizusawa Industrial Chemicals, Ltd. | Process for preparation of synthetic crystalline zinc silicate mineral having a sauconite, willemite or hemimorphite structure |
| CN101402459A (en) * | 2007-10-01 | 2009-04-08 | 中国科学院合肥物质科学研究院 | Porous zinc silicate and preparation method thereof |
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| US4681749A (en) * | 1984-06-22 | 1987-07-21 | Mizusawa Industrial Chemicals, Ltd. | Process for preparation of synthetic crystalline zinc silicate mineral having a sauconite, willemite or hemimorphite structure |
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| 孙彦刚: "Zn基微/纳米超结构的可控合成、表征及性能", 《中国博士学位论文全文数据库 工程科技I辑》 * |
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| CN104087289B (en) * | 2014-06-30 | 2016-01-20 | 中国石油大学(华东) | A kind of method utilizing waste silicon powder water heat transfer nanometer zinc silicate luminescent material |
| CN108428882A (en) * | 2018-04-17 | 2018-08-21 | 洛阳理工学院 | A kind of zinc silicate/carbon micro-nano hierarchical structure compound and preparation method thereof |
| CN108428882B (en) * | 2018-04-17 | 2020-08-04 | 洛阳理工学院 | Zinc silicate/carbon micro-nano hierarchical structure compound and preparation method thereof |
| CN109824055A (en) * | 2019-04-04 | 2019-05-31 | 河北工业大学 | The method for preparing nano-sheet zinc silicate compound adsorbent using iron tailings |
| CN109824055B (en) * | 2019-04-04 | 2022-06-07 | 河北工业大学 | Method for preparing nano flaky zinc silicate composite adsorbent by using iron tailings |
| CN112221503A (en) * | 2020-10-15 | 2021-01-15 | 山东科技大学 | Multi-level nano array phyllosilicate catalyst and preparation method thereof |
| CN112221503B (en) * | 2020-10-15 | 2023-01-31 | 山东科技大学 | Multi-level nano array phyllosilicate catalyst and preparation method thereof |
| CN117003253A (en) * | 2023-07-26 | 2023-11-07 | 上海师范大学 | Zinc silicate flower-shaped porous microsphere and preparation method thereof |
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