CN102976344A - Preparation method of zinc silicate nanometer material - Google Patents

Preparation method of zinc silicate nanometer material Download PDF

Info

Publication number
CN102976344A
CN102976344A CN2012105881976A CN201210588197A CN102976344A CN 102976344 A CN102976344 A CN 102976344A CN 2012105881976 A CN2012105881976 A CN 2012105881976A CN 201210588197 A CN201210588197 A CN 201210588197A CN 102976344 A CN102976344 A CN 102976344A
Authority
CN
China
Prior art keywords
reaction
zinc silicate
zinc
preparations
nanomaterials
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN2012105881976A
Other languages
Chinese (zh)
Other versions
CN102976344B (en
Inventor
张绍岩
次立杰
陆敏
杨建超
孙凤
王淑玲
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shijiazhuang University
Original Assignee
Shijiazhuang University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shijiazhuang University filed Critical Shijiazhuang University
Priority to CN201210588197.6A priority Critical patent/CN102976344B/en
Publication of CN102976344A publication Critical patent/CN102976344A/en
Application granted granted Critical
Publication of CN102976344B publication Critical patent/CN102976344B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Landscapes

  • Silicates, Zeolites, And Molecular Sieves (AREA)

Abstract

The invention discloses a preparation method of a zinc silicate nanometer material. Amorphous nanometer silicon dioxide and soluble zinc salt are used as raw materials. The preparation method comprises the following steps: (A) weighing the amorphous nanometer silicon dioxide and the soluble zinc salt according to a stoichiometric ratio so as to prepare a suspended aqueous solution, regulating pH value of the suspended aqueous solution to 5-13, and stirring the suspended aqueous solution; (B) transferring the suspended aqueous solution in the step A into a hydrothermal reaction kettle and reacting the suspended aqueous solution at 160-230 DEG C for 2-24 hours; and (C) cooling a reaction system after the reaction is finished, and washing and drying a reaction product so as to obtain the zinc silicate nanometer material. The preparation method disclosed by the invention has the advantages of mild reaction, good reproducibility, simplicity in operation and the like; and the prepared Zn2SiO4 can be widely applied to the fields of fluorescent materials, catalytic degradation, adsorbing materials and so on.

Description

A kind of zinc silicate preparations of nanomaterials method
Technical field
The present invention relates to the synthetic field of inorganic functional nano material, a kind of zinc silicate preparations of nanomaterials method particularly, it adopts one step of hydrothermal method to form nano material, and technique is simple, flow process is short.
Background technology
Zinc silicate (Zn 2SiO 4) be a kind of important inorganic materials, be widely used in the fields such as fluorescent material, sorbent material, glass additive, coating.Especially zinc silicate has the advantages such as environmental compatibility is strong, chemical stability good, moisture resistance is strong, be easy to prepare, cheap as the luminous host material, receives much attention in luminescent material research.
At present, the synthetic method of zinc silicate material mainly is high-temperature solid phase reaction method, is about to ZnO and SiO 2Mix afterwards roasting acquisition (Y. Wang, Y. Hao, L. H. Yuwen, J. Alloy. Compd. 2006,425,339-342 in the hot environment more than 1000 ℃ by stoichiometric ratio; A. Morell, N. Elkhiati, J. Electrochem. Soc. 1993,140,2019-2022); Also have adopt sol-gel method obtain behind the precursor again through high-temperature heat treatment obtain (M. S. Kwon, C. J. Kim, H. L. Park, T. W. Kim, H. S. Lee, J. Mater. Sci. 2005,40,4089-4091).These methods all need hot environment, and reaction process exists the energy consumption height, fires long shortcoming of cycle; In addition, through the product that high-temperature heat treatment obtains, its moiety and particle size are wayward, and pattern is also irregular, and these shortcomings have restricted the performance of material to a certain extent.
In recent years, along with the development of Materials science and nanotechnology, nano material is because its unique microtexture demonstrates impayable advantage on its performance gradually.Compare with traditional bulk material, the particle diameter of nano material is little, specific surface area is large, in use can show better properties, and is of great advantage to the application of material.At present, the research for preparing the aspect about hydrothermal method acquisition zinc silicate nano material is also very limited at home and abroad, mostly needs to introduce tensio-active agent (X. Yu, Y. H. Wang, J. Nanosci. Nanotechno. 2010,10,1-4; J. X. Wan, Z. H. Wang, X. Y. Chen, L. Mu, W. C. Yu, Y. T. Qian, J. Lumin. 2006,121,32-38), organic formwork agent (G. Q. Xu, J. Q. Liu, Z. X. Zheng, Y. C. Wu, Chin. J. Lumin. 2011,32, the additive such as 550-554), or under 280 ℃ high temperature, could obtain (H. F. Wang through long-time reaction, Y. Q. Ma, G. S. Yi, D. P. Chen, Mater. Chem. Phys. 2003,82,414-418), these methods have increased preparation cost greatly, also are unfavorable for industrial production simultaneously.Therefore: explore the low temperature controllable preparation method of zinc silicate nano material, be of great significance for the application tool of zinc silicate material.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of zinc silicate preparations of nanomaterials method, and it adopts hydrothermal method one-step synthesis nanometer zinc silicate, and the method temperature of reaction is low, technique is simple, product pattern and size are easy to control.
For solving the problems of the technologies described above, the technical scheme that the present invention takes is:
A kind of zinc silicate preparations of nanomaterials method, take the amorphous nano silicon-dioxide of stoichiometric ratio and soluble zinc salt as raw material, regulate the aqueous suspension pH to 5-13 of above-mentioned raw materials, then adopt hydrothermal method at 150-230 ℃ of reaction 2-24h, get the zinc silicate nano material.
Particularly, above-mentioned preparation method comprises the steps:
Steps A, take by weighing amorphous nano silicon-dioxide and the soluble zinc salt of stoichiometric ratio, be mixed with aqueous suspension, and adjust pH stirs to 5-13;
Step B, the aqueous suspension in the steps A is changed in the hydrothermal reaction kettle, in 150-230 ℃ of reaction 2-24 hour;
Step C, the reaction system that will react complete are cooled off, and reaction product gets the zinc silicate nano material through washing, drying.
Preferably, described soluble zinc salt is zinc nitrate, zinc sulfate or zinc chloride.
Soluble zinc salt is zinc nitrate, zinc sulfate or zinc chloride.
In the steps A in the aqueous suspension concentration of soluble zinc salt be 0.1-1mol/L.Zinc salt dissolves, and silicon-dioxide is non-water-soluble, has formed the aqueous suspension that contains 0.1-1 mol/L soluble zinc salt.
Preferably, regulate the pH value with NaOH or the KOH aqueous solution, stir 20-40min.Can not regulate the pH value with ammoniacal liquor among the present invention, can generate Zn (OH) 2Precipitation.
The preferred 200-220 of temperature of reaction ℃, when temperature of reaction was lower than 150 ℃, the product of generation was tested through XRD, and it is more to contain impurity.
Difference water and absolute ethanol washing are 3-5 time among the step C.Remaining foreign ion in the washing reaction system.
In the technique scheme, take stoichiometric amorphous nano silicon-dioxide and soluble zinc salt as raw material, take water as medium, adopt one step hydro thermal method can make grain size as the zinc silicate nano material of 20-300nm, need not use any tensio-active agent or organic formwork agent in the reaction process, operation is simple, experiment condition is controlled, good reproducibility.
The beneficial effect that adopts technique scheme to produce is: the advantage that (1) temperature of reaction of the present invention is low, reaction conditions is gentle, and technique is simple, good reproducibility, product crystal property are excellent, energy consumption of reaction is low, and environmental protection is suitable for industrialized scale production; (2) the present invention adopts one step hydro thermal method to realize the controlled preparation of low temperature of zinc silicate, adopts wet method synthetic, has realized the mixing on molecular level of zinc, silicon, oxygen, and product composition is controlled easily, even size distribution; (3) can control pattern and the size of zinc silicate Nano/micron material by reaction conditionss such as control temperature of reaction, reaction times, system pH and raw materials.
Description of drawings
Fig. 1 and Fig. 2 are respectively the Zn that embodiment 1 makes 2SiO 4The X-ray powder diffraction of nano particle (XRD) figure and scanning electron microscope analysis (SEM) figure;
Fig. 3 and Fig. 4 are respectively the Zn that embodiment 2 makes 2SiO 4The XRD figure of nanometer rod and SEM figure;
Fig. 5 and Fig. 6 are respectively the Zn that embodiment 3 makes 2SiO 4The XRD figure of nanometer rod and SEM figure;
Fig. 7 and Fig. 8 are respectively the Zn that embodiment 4 makes 2SiO 4The XRD figure of nanometer stub and SEM figure;
Fig. 9 and Figure 10 are respectively the Zn that embodiment 5 makes 2SiO 4The XRD figure of nanometer stub and SEM figure.
Embodiment
Embodiment 1
A kind of zinc silicate preparations of nanomaterials method take amorphous nano silicon-dioxide and soluble zinc salt as raw material, specifically comprises the steps:
Under steps A, the room temperature, take by weighing the amorphous nano SiO that the 2mmol diameter is about 200nm 2Add to the Zn (NO of 10mL 0.4mol/L 3) 26H 2In the O solution, stir 10 min, form aqueous suspension, then with the NaOH solution of 1mol/L the pH value of reaction system is transferred to 5, continuation stirring 30min;
Step B, the aqueous suspension in the steps A is changed in the 25 mL hydrothermal reaction kettles, be placed on after the sealing in the thermostat container, 220 ℃ of hydro-thermal reactions 24 hours;
Step C, reaction are cooled to room temperature with reaction system after complete, with the reaction product centrifugation, then use respectively deionized water and dehydrated alcohol difference washing reaction product each 5 times, remove foreign ion, then the product after will washing is 60 ℃ of vacuum-drying 4h in vacuum drying oven, obtain Zn 2SiO 4Nano particle.
The Zn that present embodiment makes 2SiO 4The XRD spectra of nano particle as shown in Figure 1, the intensity of its diffraction peak and position and Zn2SiO4 standard card (JCPDS-ICDD No. 37-1485) match, and do not have the dephasign diffraction peak, illustrate to have obtained the higher Zn of purity 2SiO 4Nano particle.
Zn 2SiO 4The scanning electron microscope analysis of nano particle (Fig. 2) shows: the Zn of present embodiment preparation 2SiO 4Be comprised of the uniform nano particle of a large amount of diameters, particle diameter is about 50nm.
Present embodiment has prepared the Zn that particle diameter is about 50nm with lower temperature, simple technique 2SiO 4, do not add any tensio-active agent or other dispersion agents in the reaction process, simple to operate, impurity is few, condition be easy to control.
Embodiment 2
Under steps A, the room temperature, take by weighing the amorphous nano SiO that the 2mmol diameter is about 200nm 2Add to the Zn (NO of 10 mL, 0.4 mol/L 3) 26H 2In the O solution, stir 10min, form aqueous suspension, then with the NaOH solution of 1mol/L the pH value of reaction system is transferred to 9 after, continuation stirring 30min;
Step B, the aqueous suspension in the steps A is changed in the 25 mL hydrothermal reaction kettles, be placed on after the sealing in the thermostat container, 220 ℃ of hydro-thermal reactions 24 hours;
Step C, reaction are cooled to room temperature with reaction system after complete, with the reaction product centrifugation, then use respectively deionized water and dehydrated alcohol difference washing reaction product each 5 times, remove foreign ion, then the product after will washing is 60 ℃ of vacuum-drying 4h in vacuum drying oven, obtain Zn 2SiO 4Nanometer rod.
The Zn that present embodiment makes 2SiO 4The XRD spectra of nanometer rod as shown in Figure 3, the intensity of its diffraction peak and position and Zn 2SiO 4Standard card (JCPDS-ICDD No. 37-1485) matches; Scanning electron microscope analysis (Fig. 4) shows: product is to be made of a large amount of nanometer rod, and the diameter of single nanometer rod is about 100 nm, and length is about 500nm, and length-to-diameter ratio is about 5, and the size of nanometer rod is more even.
Embodiment 3
Under steps A, the room temperature, take by weighing the amorphous nano SiO that the 2mmol diameter is about 200nm 2Add to the Zn (NO of 10mL 0.4 mol/L 3) 26H 2In the O solution, stir 20 min, form aqueous suspension, then with the NaOH solution of 2mol/L the pH value of reaction system is transferred to 13 after, continuation stirring 30min;
Step B, the aqueous suspension in the steps A is changed in the 25 mL hydrothermal reaction kettles, be placed on after the sealing in the thermostat container, 220 ℃ of hydro-thermal reactions 24 hours;
Step C, reaction are cooled to room temperature with reaction system after complete, with the reaction product centrifugation, then use respectively deionized water and dehydrated alcohol difference washing reaction product repeatedly, remove foreign ion, then the product after will washing is 60 ℃ of vacuum-drying 4h in vacuum drying oven, obtain Zn 2SiO 4Sub-micrometer rod.
The Zn of present embodiment preparation 2SiO 4The XRD spectra of sub-micrometer rod as shown in Figure 5.The intensity of its diffraction peak and position and Zn 2SiO 4Standard card (JCPDS-ICDD No. 37-1485) matches; Scanning electron microscope analysis (Fig. 6) shows: product is to be made of a large amount of finely disseminated sub-micrometer rods, and the surface of sub-micrometer rod is more smooth, and the diameter of single sub-micrometer rod is about 200 nm, and length is about 2-4 μ m, and length-to-diameter ratio is 10-20, and size is more even.
Embodiment 4
Under steps A, the room temperature, claim the 2mmol diameter to be about the amorphous nano SiO of 200nm 2Add to the Zn (NO of 5mL 0.8mol/L 3) 26H 2In the O solution, stir 10 min, form aqueous suspension, then with the NaOH solution of 1mol/L the pH value of reaction system is transferred to 9 after, continuation stirring 30min;
Step B, the aqueous suspension in the steps A is changed in the 25 mL hydrothermal reaction kettles, be placed on after the sealing in the thermostat container, 220 ℃ of hydro-thermal reactions 2 hours;
Step C, reaction are cooled to room temperature with reaction system after complete, with the reaction product centrifugation, then use respectively deionized water and dehydrated alcohol difference washing reaction product repeatedly, remove foreign ion, then the product after will washing is 60 ℃ of vacuum-drying 4h in vacuum drying oven, obtain Zn 2SiO 4The nanometer stub.
The Zn that present embodiment is prepared 2SiO 4The XRD spectra of nanometer stub as shown in Figure 7.The intensity of its diffraction peak and position and Zn 2SiO 4Standard card (JCPDS-ICDD No. 37-1485) matches; Scanning electron microscope analysis (Fig. 8) shows: product is to be made of a large amount of nanometer stubs, and the surface of nanometer stub is more smooth, and the diameter of single nanometer rod is about 100 nm, and length is about 200 nm, and length-to-diameter ratio is about 2, size uniform, favorable dispersity.
Embodiment 5
Under steps A, the room temperature, take by weighing the amorphous nano SiO that the 2mmol diameter is about 200nm 2Add to the Zn (NO of 10mL 0.4mol/L 3) 26H 2In the O solution, stir 10 min, form aqueous suspension, then with the NaOH solution of 1mol/L the pH value of reaction system is transferred to 9 after, continuation stirring 30min;
Step B, the aqueous suspension in the steps A is changed in the 25 mL hydrothermal reaction kettles, be placed on after the sealing in the thermostat container, 160 ℃ of hydro-thermal reactions 24 hours;
Step C, reaction are cooled to room temperature with reaction system after complete, with the reaction product centrifugation, then use respectively deionized water and dehydrated alcohol difference washing reaction product repeatedly, remove foreign ion, then the product after will washing is 60 ℃ of vacuum-drying 4h in vacuum drying oven, obtain Zn 2SiO 4The nanometer stub.
The Zn of present embodiment preparation 2SiO 4The XRD spectra of nanometer stub as shown in Figure 9.The intensity of its diffraction peak and position and Zn 2SiO 4Standard card (JCPDS-ICDD No. 37-1485) matches; Scanning electron microscope analysis (Figure 10) shows: product is to be made of a large amount of nanometer stubs, and the surface of nanometer stub is more smooth, and the diameter of single nanometer rod is about 100 nm, and length is about 200 nm, and length-to-diameter ratio is about 2, size uniform, favorable dispersity.
Embodiment 6
With reference to the synthetic Zn of the method steps of embodiment 1 2SiO 4Material, different is:
Raw material is the ZnSO of 10mL0.4mol/L 4, reaction conditions is: at 200 ℃ of reaction 10h, transfer pH to 10.
The Zn of present embodiment preparation 2SiO 4Be the nano particle of diameter at 80 ~ 120nm, size uniform.XRD figure spectrum and Zn 2SiO 4Standard card (JCPDS-ICDD No. 37-1485) matches.
Embodiment 7
With reference to the synthetic Zn of the method steps of embodiment 1 2SiO 4Material, different is:
Raw material is the ZnCl of 10mL0.4mol/L 2, reaction conditions is: at 180 ℃ of reaction 12h, transfer pH to 9.
The Zn of present embodiment preparation 2SiO 4For diameter is about 120nm, length is about 250nm, and length-to-diameter ratio is about 2 nanometer rod, size uniform, favorable dispersity.XRD figure spectrum and Zn 2SiO 4Standard card (JCPDS-ICDD No. 37-1485) matches.
In sum, the present invention adopts simple technique, lower reaction conditions to prepare size uniform, nano material that pattern is good, is suitable for suitability for industrialized production.

Claims (9)

1. zinc silicate preparations of nanomaterials method, it is characterized in that take the amorphous nano silicon-dioxide of stoichiometric ratio and soluble zinc salt as raw material, regulate the aqueous suspension pH to 5-13 of above-mentioned raw materials, then adopt hydrothermal method at 150-230 ℃ of reaction 2-24h, get the zinc silicate nano material.
2. zinc silicate preparations of nanomaterials method according to claim 1 is characterized in that described method comprises the steps:
Steps A, take by weighing amorphous nano silicon-dioxide and the soluble zinc salt of stoichiometric ratio, be mixed with aqueous suspension, and adjust pH stirs to 5-13;
Step B, the aqueous suspension in the steps A is changed in the hydrothermal reaction kettle, in 150-230 ℃ of reaction 2-24 hour;
Step C, the reaction system that will react complete are cooled off, and reaction product gets the zinc silicate nano material through washing, drying.
3. zinc silicate preparations of nanomaterials method according to claim 1 and 2 is characterized in that described soluble zinc salt is zinc nitrate, zinc sulfate or zinc chloride.
4. zinc silicate preparations of nanomaterials method according to claim 1 and 2, the concentration that it is characterized in that soluble zinc salt in the aqueous suspension is 0.1-1mol/L.
5. zinc silicate preparations of nanomaterials method according to claim 1 and 2 is characterized in that regulating the pH value with NaOH or the KOH aqueous solution, stirs 20-40min.
6. zinc silicate preparations of nanomaterials method according to claim 1 and 2 is characterized in that temperature of reaction is 200-220 ℃.
7. zinc silicate preparations of nanomaterials method according to claim 1 is characterized in that distinguishing among the step C water and absolute ethanol washing 3-5 time.
8. zinc silicate preparations of nanomaterials method according to claim 1 is characterized in that the drying conditions among the step C is: 60-80 ℃ vacuum-drying 2-4 hour.
9. zinc silicate preparations of nanomaterials method according to claim 1, the particle size range that it is characterized in that the zinc silicate nano material is 20-300nm.
CN201210588197.6A 2012-12-29 2012-12-29 Preparation method of zinc silicate nanometer material Expired - Fee Related CN102976344B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201210588197.6A CN102976344B (en) 2012-12-29 2012-12-29 Preparation method of zinc silicate nanometer material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201210588197.6A CN102976344B (en) 2012-12-29 2012-12-29 Preparation method of zinc silicate nanometer material

Publications (2)

Publication Number Publication Date
CN102976344A true CN102976344A (en) 2013-03-20
CN102976344B CN102976344B (en) 2015-04-15

Family

ID=47850764

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201210588197.6A Expired - Fee Related CN102976344B (en) 2012-12-29 2012-12-29 Preparation method of zinc silicate nanometer material

Country Status (1)

Country Link
CN (1) CN102976344B (en)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104383873A (en) * 2014-11-13 2015-03-04 中国科学院兰州化学物理研究所盱眙凹土应用技术研发中心 Method for preparing composite adsorbent by utilizing low-grade attapulgite clay
CN104447834A (en) * 2014-11-25 2015-03-25 廊坊师范学院 Preparation method for nano methyl zinc silicate
CN108047795A (en) * 2018-01-02 2018-05-18 华东理工大学 A kind of zinc silicate anti-corrosion paint with warning function
IT201700122793A1 (en) * 2017-10-27 2019-04-27 Bridgestone Corp NANOMATERIALS BASED ON SILICA AS SUBSTITUTES OF THE ZNO IN RUBBER COMPOUNDS AND THEIR PREPARATION
CN109796021A (en) * 2019-04-04 2019-05-24 河北工业大学 Utilize the method for iron tailings preparation ellipsoid zinc silicate compound adsorbent
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
CN117003253A (en) * 2023-07-26 2023-11-07 上海师范大学 Zinc silicate flower-shaped porous microsphere and preparation method thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102502672A (en) * 2011-10-26 2012-06-20 中国科学院化学研究所 Layered multi-stage zinc silicate and preparation method and application thereof

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102502672A (en) * 2011-10-26 2012-06-20 中国科学院化学研究所 Layered multi-stage zinc silicate and preparation method and application thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
许海艇、徐光青、郑治祥、吴玉程: "不同硅源对水热合成Zn_2SiO_4:Mn荧光材料形貌及性能的影响", 《过程工程学报》 *

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104383873A (en) * 2014-11-13 2015-03-04 中国科学院兰州化学物理研究所盱眙凹土应用技术研发中心 Method for preparing composite adsorbent by utilizing low-grade attapulgite clay
CN104383873B (en) * 2014-11-13 2016-08-24 中国科学院兰州化学物理研究所盱眙凹土应用技术研发中心 Method for preparing composite adsorbent by using low-grade attapulgite clay
CN104447834A (en) * 2014-11-25 2015-03-25 廊坊师范学院 Preparation method for nano methyl zinc silicate
CN104447834B (en) * 2014-11-25 2017-03-22 廊坊师范学院 Preparation method for nano methyl zinc silicate
IT201700122793A1 (en) * 2017-10-27 2019-04-27 Bridgestone Corp NANOMATERIALS BASED ON SILICA AS SUBSTITUTES OF THE ZNO IN RUBBER COMPOUNDS AND THEIR PREPARATION
WO2019082069A1 (en) * 2017-10-27 2019-05-02 Bridgestone Corporation Silica based nanomaterials as substitutes for zno in rubber compounds and preparation thereof
CN108047795A (en) * 2018-01-02 2018-05-18 华东理工大学 A kind of zinc silicate anti-corrosion paint with warning function
CN109796021A (en) * 2019-04-04 2019-05-24 河北工业大学 Utilize the method for iron tailings preparation ellipsoid zinc silicate compound adsorbent
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
CN109796021B (en) * 2019-04-04 2022-04-05 河北工业大学 Method for preparing ellipsoidal zinc silicate composite adsorbent by 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
CN117003253A (en) * 2023-07-26 2023-11-07 上海师范大学 Zinc silicate flower-shaped porous microsphere and preparation method thereof

Also Published As

Publication number Publication date
CN102976344B (en) 2015-04-15

Similar Documents

Publication Publication Date Title
CN102976344B (en) Preparation method of zinc silicate nanometer material
CN104148047B (en) Macro preparation method for carbon doped zinc oxide-based visible-light catalyst
CN102515255A (en) Method for preparing zinc sulfide nanospheres
CN105502421A (en) Preparation method of zinc silicate hollow micron ball
CN102491404A (en) Copper oxide micro-nano composite structural material and preparation method thereof
CN103435097B (en) Preparation method and application of nano zirconia
CN101613121A (en) A kind of preparation method of ellipsoid-shaped zinc oxide
Zou et al. Ultrasound-assisted synthesis of CuO nanostructures templated by cotton fibers
CN103833080A (en) Preparation method for cadmium molybdate porous spheres
CN111569879B (en) Method for preparing silicate/carbon composite material by using attapulgite and application thereof
CN101319404A (en) Method for preparation of hollow spherical cadmium sulfide nanocrystalline
CN103466688B (en) A kind of method for preparing ZnS nanosheet
CN102897723A (en) Hydrothermal method for preparing selenium-copper-based nano-crystals
CN105752957B (en) Using the method for preparing nano-scale rare earth phosphate phosphor from sacrifice template method
CN1321942C (en) Method for preparing Nano crystal of metal oxide of anti agglomeration
CN102320659B (en) Method for synthesizing lanthanum-vanadate nano material by adopting microwave-radiation method
CN101774603B (en) Preparation method of mesoporous magnesium borate microsphere
CN109338466B (en) Preparation of single crystal Fe2O3Method for self-assembling nano-particle into elliptical micro-nano structure
CN103482672B (en) Preparation method of hexagonal-prism-shaped Sm(OH)3 nanocrystalline
CN101648726B (en) Hydrothermal synthesis method of LuO(OH) nanorods and Lu2O3 nanorods luminescent powder
CN102923759A (en) Method for preparing pure-phase monodisperse ZnS nanocrystalline by using diethylene glycol serving as solvent
CN104071826B (en) Preparation method of modified nanometer ZnO powder
Huang et al. Surfactant-assisted synthesis and luminescent properties of Gd2O3: Eu3+ core–shell microspheres
CN104649329B (en) A kind of α-Fe2o3the preparation method of nanoparticle
CN102424417A (en) Method for preparing stabilized aluminium titanate superfine powder by sol-gel technology under low temperature and product prepared therefrom

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20150415

Termination date: 20191229

CF01 Termination of patent right due to non-payment of annual fee