CN102583514A - Nano linear calcium titanate and synthesis method thereof - Google Patents
Nano linear calcium titanate and synthesis method thereof Download PDFInfo
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- CN102583514A CN102583514A CN2012100013021A CN201210001302A CN102583514A CN 102583514 A CN102583514 A CN 102583514A CN 2012100013021 A CN2012100013021 A CN 2012100013021A CN 201210001302 A CN201210001302 A CN 201210001302A CN 102583514 A CN102583514 A CN 102583514A
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Abstract
The invention discloses nano linear calcium titanate and a synthesis method thereof. The synthesis method for the nano linear calcium titanate comprises the following steps of: 1) dispersing titanium dioxide in a strong alkali solution, and performing a hydro-thermal reaction with stirring to obtain a white deposit; 2) washing the white deposit by using water until the white deposit is neutral or weakly alkaline, dispersing the white deposit in a soluble calcium salt solution, controlling the temperature and the pH value of the system, and performing ion exchange reaction to obtain a calcium titanate deposit; and 3) performing centrifugal washing on the calcium titanate deposit until the calcium titanate deposit is neutral, and drying and baking the calcium titanate deposit to obtain the nano linear calcium titanate. The synthesis method for the nano linear calcium titanate is mild in reaction condition, simple in operation, rich in raw material source and low in cost, so that the synthesis method is suitable for mass production; and the synthesized nano linear calcium titanate is a solid alkali with a large specific area, has high ecological biocompatibility, and is expected to be applied in the fields of heavy metal ion contaminated waste water purification, ester exchange reaction catalysis, sclerous tissue repair and replacement and the like.
Description
Technical field
The present invention relates to a kind of calcium titanate and compound method thereof, specifically relate to the method for a kind of nanometer wire calcium titanate and synthetic this nanometer wire calcium titanate.
Background technology
Since carbon nanotube came to light, monodimension nanometer material had evoked scientists with its particular structure (tubulose, small-bore, bigger serface) and wide application prospect (photoelectricity, sensing, catalysis, single-electronic transistor, molecule suction pipe, matrix material) and has studied interest greatly.Synthesizing, characterize and using of monodimension nanometer material become important research direction in the field of nanometer material technology; Wherein representative one type of nano material is an one dimension metatitanic acid salt nano material; It adopts the porous anodic alumina template method at first to make titania nanotube in Hoyer in 1996 and Patrick [Langmuir, 1996,12:1411-1413]; Subsequently; [Langmuir, 1998,14 (12): 3160-3163] such as Kasuga T adopted hydrothermal method to synthesize protonated titanate nanotube in 1998.
At present, the compound method of monodimension nanometer material titanate mainly contains template, anonizing, hydrothermal method.Template is to obtain ordered nano-structure one of effective means the most, but not only the template synthesis technique is complicated for this method, and the caliber of gained nanotube is big, thickness of pipe, specific surface area are little; And the aperture of pipe receives the restriction of pore size of template and pattern, can be adsorbed in template preferably in order to make resultant, and is also high to the degree of cleaning requirement of template surface; And test rear pattern plate all can destroy at every turn; Can't reuse, cause the synthetic cost of material too high, be difficult to carry out large-scale commercial prodn.Anonizing is the one dimension TiO that pure titanium sheet is obtained different-shape and degree of crystallization in electrolytic solution through anodic oxidation
2Nano material, voltage and electrolytic solution affect the pattern and the size of nanotube in whole process, and the electrolytic solution influence factor is more, is not easy allotment, thus limited its scale operation.Adopt hydrothermal method synthesizing titanate monodimension nanometer material; Not only synthetic monodimension nanometer material complete shape and appearance, caliber is little, tube wall is thin, specific surface area is big; And have that raw material sources are abundant, technology simple, low cost and other advantages, thereby become the focus of present research.
Titanate product category as uhligite is various, can be divided into alkali metal titanate, titanates of alkali-earth metals, rare earth metal titanate etc. by its composition.Titanates of alkali-earth metals MTiO
3(M=Ca, Sr Ba) have unique electricity, optics and chemical property, have caused people's very big interest in many technical applications.Though China's titanium aboundresources; Standing stock are first of the world; For China's titanium hydrochlorate industrial expansion has been created favourable condition; But China is also very backward compared with developed countries at research and development titanate series products, and this is extremely unbecoming with the such titanium resource big country of China, and therefore research seems very urgent to the titanate Products Development.For these reasons, we have proposed a kind of compound method of nanometer wire calcium titanate.
Summary of the invention
Main purpose of the present invention provides a kind of compound method of nanometer wire calcium titanate, and the nanometer wire calcium titanate through compound method of the present invention preparation.
The compound method of nanometer wire calcium titanate disclosed by the invention may further comprise the steps:
A) with under white titanium pigment and the stirring of certain density strong base solution, certain temperature hydro-thermal reaction certain hour generates white precipitate, and white precipitate is washed to neutrality or approaching neutral, gets white precipitate;
B) under the proper temperature condition; In the white precipitate that step a makes, add certain density solubility calcium salts solution, the amount of the soluble calcium salt of adding is slightly larger than 1 by the Ca/Ti mol ratio and calculates, under the certain pH; Stir ion exchange reaction certain hour down, get white calcium titanate deposition;
C) with calcium titanate washing of precipitate to the inclusion-free ion of the white of gained, and after being neutrality, after drying, proper temperature roasting certain hour, the cooling nanometer wire calcium titanate.
White titanium pigment is CP or analytical pure among the above-mentioned steps a, preferred analytical pure.Highly basic is sodium hydroxide or Pottasium Hydroxide, preferred sodium hydroxide.
The concentration of strong base solution is 5～15mol/L among the above-mentioned steps a, preferred 8～12mol/L.
The temperature of hydro-thermal reaction is 150～250 ℃ among the above-mentioned steps a, preferred 160～220 ℃.
The time of thermal response is 15～72h, preferred 24～48h.
Soluble calcium salt is selected from CaCl among the above-mentioned steps b
2, Ca (NO
3)
2, Ca (AC)
2In any one, preferred CaCl
2Perhaps Ca (NO
3)
2The concentration of solubility calcium salts solution is 10～50g/L, preferred 20～30g/L.The pH value of above-mentioned steps b intermediate ion permutoid reaction is 5.0～8.5, preferred 5.5～7.5.The temperature of ion exchange reaction is 30～100 ℃, preferred 50～80 ℃.The time of ion exchange reaction is 60～300min, preferred 120～240min.
Maturing temperature is 350～800 ℃ among the above-mentioned steps c, preferred 450～750 ℃.Roasting time is 120～360min, preferred 180～240min.
Compared with prior art, above-mentioned disclosed method has following advantage:
One of outstanding advantage of the present invention is to choose raw material and is easy to get, and low-cost white titanium pigment is the titanium source, and the titanium source that avoids the use of expensive solubility is a raw material, thereby greatly reduces synthetic cost.
Two of outstanding advantage of the present invention is to adopt the nanometer wire titanate presoma of hydrothermal method synthesizing one-dimensional structure, has avoided the use tensio-active agent, is the compound method of a kind of green, economy, environmental protection.
Three of outstanding advantage of the present invention is that the nanometer wire titanate with one-dimentional structure is a precursor, carries out ion exchange reaction at low temperatures with the calcium salt of solubility, has avoided high temperature solid state reaction, thus the energy consumption of greatly reducing.
Four of outstanding advantage of the present invention is that synthesis technique is simple, and is not high to equipment requirements, can realize producing in batches, thereby satisfy large-scale industrial production.
Five of outstanding advantage of the present invention is that synthetic nanometer wire calcium titanate is uniform white powder, the filament shape that synthetic nanometer wire calcium titanate is evenly distributed at sem observation, and diameter is about 1～10nm, and length is about 1～2.5 μ m.Institute's synthetic nanometer wire calcium titanate is a kind of solid base with high-specific surface area, and the ecologic biological consistency is excellent, is expected to obtain to use in fields such as heavy-metal pollution purification of waste water, transesterification reaction catalysis and hard tissue repair and replacements.
Description of drawings
Below in conjunction with accompanying drawing and embodiment the present invention is done further detailed explanation.
Fig. 1 is the synthesis technique schematic flow sheet of nanometer wire calcium titanate.
Fig. 2 is the X-ray powder diffraction spectrogram (XRD spectrum) of nanometer wire calcium titanate.
Fig. 3 be nanometer wire calcium titanate electron scanning micrograph (the SEM photo, a left side figure be 5000 times of photos, the right side figure be 20000 times of photos, be left picture frame inner compartment enlarged view).
Fig. 4 is the electronic energy spectrum (EDS spectrum) of nanometer wire calcium titanate.
Embodiment
Provide a kind of embodiment of indefiniteness of nanometer wire calcium titanate compound method produced according to the present invention below.
Embodiment 1
1) preparation of strong base solution: accurately take by weighing the analytically pure sodium hydroxide of 100 grams, be dissolved in the 500mL deionized water strong base solution A, the amount of substance concentration of strong base solution A is 5mol/L;
2) hydro-thermal reaction: accurately take by weighing the analytically pure white titanium pigment of 0.8 gram; After the strong base solution A of adding 30mL stirs; Be transferred in the stainless reaction kettle, stirred hydro-thermal reaction 15 hours in 150 ℃ reaction conditions lower magnetic forces, the cooling after scouring is to the approaching neutral white precipitate B that gets;
3) preparation of solubility calcium salts solution: accurately take by weighing the analytically pure Calcium Chloride Powder Anhydrous of 25 grams, be dissolved in the 500mL deionized water the soluble calcium salt solution C, the mass concentration of soluble calcium salt solution C is 50g/L;
4) ion exchange reaction: measure the soluble calcium salt solution C of 35mL, add in the above-mentioned white precipitate B, adjust pH 5.0 got white precipitate D in 60 minutes in 30 ℃ reaction conditions lower magnetic forces stirrings;
5) roasting: with deionized water centrifuge washing to inclusion-free ion and be neutral, dry back is in 350 ℃ of roastings 120 minutes with above-mentioned white precipitate D, after the cooling white nanometer wire calcium titanate powder E.
1) preparation of strong base solution: accurately take by weighing the analytically pure sodium hydroxide of 150 grams, dissolve with the 250mL deionized water in strong base solution A, the amount of substance concentration of strong base solution A is 15mol/L;
2) hydro-thermal reaction: accurately take by weighing the analytically pure white titanium pigment of 0.8 gram; After the strong base solution A of adding 30mL stirs; Be transferred in the stainless reaction kettle, stirred hydro-thermal reaction 15 hours in 250 ℃ reaction conditions lower magnetic forces, the cooling after scouring is to the approaching neutral white precipitate B that gets;
3) preparation of solubility calcium salts solution: accurately take by weighing the analytically pure Calcium Chloride Powder Anhydrous of 5 grams, be dissolved in the 500mL deionized water the soluble calcium salt solution C, the mass concentration of soluble calcium salt solution C is 10g/L;
4) ion exchange reaction: measure the soluble calcium salt solution C of 120mL, add in the above-mentioned white precipitate B, adjust pH 5.0 got white precipitate D in 60 minutes in 100 ℃ reaction conditions lower magnetic forces stirrings;
5) roasting: with deionized water centrifuge washing to inclusion-free ion and be neutral, dry back is in 800 ℃ of roastings 120 minutes with above-mentioned white precipitate D, after the cooling white nanometer wire calcium titanate powder E.
Embodiment 3
1) preparation of strong base solution: accurately take by weighing the analytically pure sodium hydroxide of 200 grams, be dissolved in the 500mL deionized water strong base solution A, the amount of substance concentration of strong base solution A is 10mol/L;
2) hydro-thermal reaction: accurately take by weighing the analytically pure white titanium pigment of 0.8 gram; After the strong base solution A of adding 30mL stirs; Be transferred in the stainless reaction kettle, stirred hydro-thermal reaction 24 hours in 180 ℃ reaction conditions lower magnetic forces, the cooling after scouring is to the approaching neutral white precipitate B that gets;
3) preparation of solubility calcium salts solution: accurately take by weighing the analytically pure Calcium Chloride Powder Anhydrous of 25 grams, be dissolved in the 500mL deionized water the soluble calcium salt solution C, the mass concentration of soluble calcium salt solution C is 50g/L;
4) ion exchange reaction: measure the soluble calcium salt solution C of 35mL, add in the above-mentioned white precipitate B, adjust pH 6.0 got white precipitate D in 300 minutes in 80 ℃ reaction conditions lower magnetic forces stirrings;
5) roasting: with deionized water centrifuge washing to inclusion-free ion and be neutral, dry back is in 450 ℃ of roastings 360 minutes with above-mentioned white precipitate D, after the cooling white nanometer wire calcium titanate powder E.
1) preparation of strong base solution: accurately take by weighing the analytically pure Pottasium Hydroxide of 280 grams, be dissolved in the 500mL deionized water strong base solution A, the amount of substance concentration of strong base solution A is 10mol/L;
2) hydro-thermal reaction: accurately take by weighing the analytically pure white titanium pigment of 0.8 gram; After the strong base solution A of adding 30mL stirs; Be transferred in the stainless reaction kettle, stirred hydro-thermal reaction 48 hours in 160 ℃ reaction conditions lower magnetic forces, the cooling after scouring is to the approaching neutral white precipitate B that gets;
3) preparation of solubility calcium salts solution: accurately take by weighing the analytically pure anhydrous acetic acid calcium of 25 grams, be dissolved in the 500mL deionized water the soluble calcium salt solution C, the mass concentration of soluble calcium salt solution C is 50g/L;
4) ion exchange reaction: measure the soluble calcium salt solution C of 35mL, add in the above-mentioned white precipitate B, adjust pH 7.0 got white precipitate D in 180 minutes in 60 ℃ reaction conditions lower magnetic forces stirrings;
5) roasting: with deionized water centrifuge washing to inclusion-free ion and be neutral, dry back is in 600 ℃ of roastings 150 minutes with above-mentioned white precipitate D, after the cooling white nanometer wire calcium titanate powder E.
Embodiment 5
1) preparation of strong base solution: accurately take by weighing the analytically pure Pottasium Hydroxide of 140 grams, be dissolved in the 500mL deionized water strong base solution A, the amount of substance concentration of strong base solution A is 5mol/L;
2) hydro-thermal reaction: accurately take by weighing the analytically pure white titanium pigment of 0.8 gram; After the strong base solution A of adding 50mL stirs; Be transferred in the stainless reaction kettle, stirred hydro-thermal reaction 24 hours in 200 ℃ reaction conditions lower magnetic forces, the cooling after scouring is to the approaching neutral white precipitate B that gets;
3) preparation of solubility calcium salts solution: accurately take by weighing the analytically pure anhydrous acetic acid calcium of 5 grams, be dissolved in the 500mL deionized water the soluble calcium salt solution C, the mass concentration of soluble calcium salt solution C is 10g/L;
4) ion exchange reaction: measure the soluble calcium salt solution C of 120mL, add in the above-mentioned white precipitate B, adjust pH 8.5 got white precipitate D in 120 minutes in 50 ℃ reaction conditions lower magnetic force stirring;
5) roasting: with above-mentioned white precipitate D with deionized water centrifuge washing to inclusion-free ion and be neutral, dry back in 750 ℃ of roastings 180 minutes, after the cooling white nanometer wire calcium titanate powder E.
1) preparation of strong base solution: accurately take by weighing the analytically pure Pottasium Hydroxide of 224 grams, be dissolved in the 500mL deionized water strong base solution A, the amount of substance concentration of strong base solution A is 8mol/L;
2) hydro-thermal reaction: accurately take by weighing the analytically pure white titanium pigment of 0.8 gram; After the strong base solution A of adding 35mL stirs; Be transferred in the stainless reaction kettle, stirred hydro-thermal reaction 36 hours in 170 ℃ reaction conditions lower magnetic forces, the cooling after scouring is to the approaching neutral white precipitate B that gets;
3) preparation of solubility calcium salts solution: accurately take by weighing the analytically pure anhydrous acetic acid calcium of 15 grams, be dissolved in the 500mL deionized water the soluble calcium salt solution C, the mass concentration of soluble calcium salt solution C is 30g/L;
4) ion exchange reaction: measure the soluble calcium salt solution C of 40mL, add in the above-mentioned white precipitate B, adjust pH 7.5 got white precipitate D in 240 minutes in 40 ℃ reaction conditions lower magnetic forces stirrings;
5) roasting: with above-mentioned white precipitate D with deionized water centrifuge washing to inclusion-free ion and be neutral, dry back in 500 ℃ of roastings 300 minutes, after the cooling white nanometer wire calcium titanate powder E.
More than through specific embodiment the present invention has been carried out the explanation of details, but the present invention is not limited only to these embodiment.Under the prerequisite that does not break away from the present invention's design, more other embodiments can also be arranged.Protection scope of the present invention is confirmed by the scope of claim.The above; Be merely the preferable embodiment of the present invention, but protection scope of the present invention is not limited thereto, any technician who is familiar with the present technique field is in the technical scope that the present invention discloses; The variation that can expect easily or replacement all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claims.
Claims (9)
1. the compound method of a nanometer wire calcium titanate comprises the steps:
A) hydro-thermal reaction: divided titanium dioxide is dispersed in the alkaline solution of 5～15mol/L; Adding in the 100ml alkali lye and be no more than the 2g white titanium pigment, after the stirring, is under 150～250 ℃ the condition in temperature; Hydro-thermal reaction 15～48 hours, the cooling after scouring is to the approaching neutral white precipitate that gets;
B) ion exchange reaction: in the white precipitate that step a makes, add the solubility calcium salts solution of 10～50g/L, the amount of the soluble calcium salt of adding is slightly larger than 1 by the Ca/Ti mol ratio and calculates, and the pH value is 5.0～8.5; Be that magnetic agitation is 60～300 minutes, obtains the calcium titanate deposition of white under 30～120 ℃ the reaction conditions in temperature;
C) roasting: the calcium titanate precipitate with deionized water of the white of gained is washed to the inclusion-free ion, and after being neutrality, dry, in 350～800 ℃ under maturing temperature, roasting 120～360 minutes, after the cooling nanometer wire calcium titanate.
2. the compound method of nanometer wire calcium titanate according to claim 1 is characterized in that, the white titanium pigment purity described in the step a is not less than CP.
3. the compound method of nanometer wire calcium titanate according to claim 1 and 2 is characterized in that, the alkaline solution described in the step a is the aqueous solution of NaOH.
4. the compound method of nanometer wire calcium titanate according to claim 1 and 2 is characterized in that, the alkaline solution described in the step a is the aqueous solution of KOH.
5. the compound method of nanometer wire calcium titanate according to claim 1 is characterized in that, getting soluble calcium salt among the step b is CaCl
2
6. the compound method of nanometer wire calcium titanate according to claim 1 is characterized in that, soluble calcium salt is Ca (NO3) among the step b
2
7. the compound method of nanometer wire calcium titanate according to claim 1 is characterized in that, soluble calcium salt is Ca (AC) among the step b
2
8. nanometer wire calcium titanate is characterized in that being the compound method preparation of nanometer wire calcium titanate according to claim 1.
9. require 8 described nanometer wire calcium titanates according to power, it is characterized in that nanometer wire calcium titanate is uniform white powder, at the filament shape that sem observation is evenly distributed, diameter is 1～10nm, and length is 1～2.5 μ m.
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Cited By (5)
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|---|---|---|---|---|
| CN105016379A (en) * | 2015-07-27 | 2015-11-04 | 昆明理工大学 | Method for preparing calcium metatitanate |
| CN106915766A (en) * | 2015-12-25 | 2017-07-04 | 兰州大学 | A kind of preparation method of butterfly-like shape calcium titanate particle |
| CN108408765A (en) * | 2018-03-20 | 2018-08-17 | 浙江大学 | A kind of preparation method of rectangular tubular calcium titanate micron particles |
| CN112108140A (en) * | 2020-08-20 | 2020-12-22 | 浙江工业大学 | Green synthetic rod-shaped CaTiO taking raw egg shells as calcium source3Method of producing a material |
| CN113880134A (en) * | 2021-10-21 | 2022-01-04 | 北京化工大学 | Preparation method and application of titanate-based hollow material |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105016379A (en) * | 2015-07-27 | 2015-11-04 | 昆明理工大学 | Method for preparing calcium metatitanate |
| CN106915766A (en) * | 2015-12-25 | 2017-07-04 | 兰州大学 | A kind of preparation method of butterfly-like shape calcium titanate particle |
| CN106915766B (en) * | 2015-12-25 | 2018-01-30 | 兰州大学 | A kind of preparation method of butterfly-like shape calcium titanate particle |
| CN108408765A (en) * | 2018-03-20 | 2018-08-17 | 浙江大学 | A kind of preparation method of rectangular tubular calcium titanate micron particles |
| CN112108140A (en) * | 2020-08-20 | 2020-12-22 | 浙江工业大学 | Green synthetic rod-shaped CaTiO taking raw egg shells as calcium source3Method of producing a material |
| CN113880134A (en) * | 2021-10-21 | 2022-01-04 | 北京化工大学 | Preparation method and application of titanate-based hollow material |
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Application publication date: 20120718 |