CN1911813A - Preparation method of calcium sulfate nanometer material - Google Patents
Preparation method of calcium sulfate nanometer material Download PDFInfo
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- CN1911813A CN1911813A CN 200610030350 CN200610030350A CN1911813A CN 1911813 A CN1911813 A CN 1911813A CN 200610030350 CN200610030350 CN 200610030350 CN 200610030350 A CN200610030350 A CN 200610030350A CN 1911813 A CN1911813 A CN 1911813A
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Abstract
The present invention belongs to the field of nanometer inorganic material technology, and is especially preparation process of nanometer calcium sulfate material. The preparation process includes the following steps: compounding calcium salt solution and sulfate solution of molar concentration 0.05-0.20 mol/l; setting the calcium salt solution in 1.5 ml in one conical flask and sulfate solution in 1.5 ml in one other conical flask; adding to each of the conical flasks C12E9 in 5 ml, n-amyl alcohol in 1 ml and cyclohexane in 40 ml via stirring to obtain two kinds of homogeneous reverse phase micellar solution separately; mixing these two kinds of reverse phase micellar solution; stilling for certain time; demulsifying separation with acetone, washing and drying to obtain nanometer luminescent calcium sulfate material, which may be nanometer particle, nanometer tube, nanometer rod or nanometer line corresponding to the stilling time of 0.8-1.5 min, 4.5-5.5 min, 8-15 hr and 100-120 hr separately.
Description
Technical field
The invention belongs to technical field of inorganic nanometer material, be specifically related to the preparation method of a kind of calcium sulfate nanometer material (nanoparticle or nanotube or nanometer rod or nano wire).
Background technology
Over nearly two, 30 years, nano material is because its particular performances has caused the research interest that researcher is dense.Usually nanoparticle is basic construction unit, and senior orderly nanostructure has nanoparticle to assemble mostly.Monodimension nanometer material is because its particular structure has very application prospects especially.Wherein, nanotube has the physics and the chemical property of a lot of excellences because of its particular structure.Thereby have boundless application prospect, thereby become one of focus that vast researcher falls over each other to study in fields such as the energy, medicine, electronics, biologies.
Yet, because the preparation of nanotube is comparatively difficult, therefore, for the nano material of other structures, also less for the achievement in research of nanotube.Wherein, major part is the carbon nanotube and the oxide nano of class graphite laminate structure.Being prepared into of non-carbon non-oxidized substance nanotube is also fewer so far.The method that can be used for preparing nanotube at present mainly contains: electrochemical process and high-temperature high-voltage reaction method.Yet all there is complicated operation in various degree in above-mentioned reaction scheme, temperature of reaction is required problems such as height, cost height, is difficult to large-scale production.Up to now, still be no more than 10 kinds for the research for preparing non-layered inorganic salt nanotube both at home and abroad.And by changing some influence factors, up to the present the report that obtains nanoparticle, nanotube, nanometer rod and nano wire respectively according to people's will in same system is not also seen as yet.
Therefore develop a kind of modern design, advanced technology, convenient and simple, with low cost, reaction conditions is gentle, can scale production non-layered inorganic salt nanoparticle or the method for nanotube or nanometer rod or nano wire significant.If can in same system, obtain nanoparticle, nanotube, nanometer rod and nano wire, realize that the integrated synthetic of above-mentioned materials will bring bigger life to the preparation of nano material according to different needs.
Summary of the invention
The objective of the invention is to propose a kind of convenient and simple, with low cost, reaction conditions is gentle, the preparation method of calcium sulfate nanometer material that can scale production.
The preparation method of the calcium sulfate nanometer material that the present invention proposes adopts reversed phase micelle soft template system assembling synthesizing inorganic salt nano material, and its concrete steps are as follows:
(1) take by weighing soluble calcium salt and vitriol, with its solution that is mixed with soluble in water respectively, wherein the mol ratio of calcium salt and vitriol is 1: 1 then, and the calcium salt soln of preparation and sulfate liquor volumetric molar concentration are respectively 0.05～0.20 mol;
(2) A: in Erlenmeyer flask, add 1.5 milliliters of calcium salt solns that are mixed with in the step (1), 5 milliliters of C respectively
12E
9, 1 milliliter of Pentyl alcohol and 40 milliliters of hexanaphthenes, stir, form the reversed phase micelle solution of transparent homogeneous;
B: add 1.5 milliliters of sulfate liquors that are mixed with in the step (1), 5 milliliters of C respectively to Erlenmeyer flask
12E
9, 1 milliliter of Pentyl alcohol and 40 milliliters of hexanaphthenes, stir, form the another kind of reversed phase micelle solution of transparent homogeneous;
(3) the two kinds of reversed phase micelle solution of A, B with gained in the step (2) mix, standing and reacting, and separation, washing, drying promptly obtain required nano material.
Among the present invention, described calcium salt is CaCl
2, Ca (NO
3)
2Deng in the soluble calcium salt any.
Among the present invention, described vitriol is Na
2SO
4, K
2SO
4Deng in the soluble sulphate any.
Among the present invention, the standing and reacting time is 0.8-1.5 minute, obtains the nanoparticle that diameter is the 10-20 nanometer.
Among the present invention, the standing and reacting time is 4.5-5.5 minute, obtains the nanotube of 50 nanometers * 400 nanometers.
Among the present invention, the standing and reacting time is 10-15 hour, obtains the nanometer rod of 60 nanometers * 5000 nanometers.
Among the present invention, the standing and reacting time is 100-120 hour, obtains the nano wire of 65 nanometers * 100000 nanometers.
Among the present invention, separating used emulsion splitter in the step (3) is acetone, and its add-on is to add the 5-10 milliliter in per 100 ml solns.
Among the present invention, described washing adopts dehydrated alcohol and distilled water alternately to clean 3-6 time.
Among the present invention, dry employing vacuum-drying, temperature is 50-70 ℃, the time is 20-60 minute.
Products therefrom of the present invention can pass through transmission electron microscope (TEM) and characterize pattern, and x-ray powder diffraction instrument (XRD) characterizes structure.
Among the present invention, XRD result shows product pure (consistent with the JCPDS card).Fluorescent spectroscopy is the result show, product has photoluminescence performance.Because the band gap of calcium sulfate is 11.5 electron-volts, so, do not absorb in the ultraviolet-visible light district.
The present invention has following advantage:
1, because the reaction system that the present invention chooses synthesizes zero dimension/one dimension in same system, hollow/solid nano material, realized synthetic material of the same race in same system, different-shape size, the nano material of different performance! Thereby greatly reduce production cost, improved the production efficiency of nano material.
2, because the present invention adopts the reversed phase micelle soft template system of stable homogeneous, induce the synthetic calcium sulfate sodium grain of rice of assembling step by step/incorporate nano material of pipe/rod/line, the product that the present invention is made has good and numerous pattern, for the exploitation of functional materials is had laid a good foundation.
3,, and, can synthesize the calcium sulfate nanometer material of different dimensions, pattern, size at room temperature by gentle easy reaction because the present invention only need adjust the reaction times.And used organic solvent can recycling in the reaction.Therefore have easy to operate, technology and simple, the free of contamination advantage of equipment.
4, the product of the present invention's preparation has performances such as good light, electricity: fluorescence strengthens.
Find that after deliberation reversed phase micelle soft template method is as a kind of effective nano material synthetic method, compare more simple and conveniently with other wet chemical methods such as sol-gel method, hydrothermal methods that and product pattern variation more just can realize at normal temperatures.Reverse micelle method is to utilize water oil two-phase under Action of Surfactant, forms stable micella, and inorganic ion generates inorganic salt by infiltration between micella and intermicellar mutual fusion combination.And under micellar soft template inducing action, produce the nano material of different-shape.
The present invention utilizes the reversed phase micelle system, selects CaCl
2And Na
2SO
4As reactant, under suitable water-oil ratio condition, when room temperature, prepare CaSO
42H
2O nanoparticle/pipe/rod/wire material.In this reaction system, regulate and control size, pattern and the dimension of product by the change reaction times.
Description of drawings
Fig. 1 is the shape appearance figure that the transmission electron microscope (TEM) of the product of embodiments of the invention 1 obtains.
Fig. 2 is the shape appearance figure that the transmission electron microscope (TEM) of the product of embodiments of the invention 2 obtains.
Fig. 3 is the shape appearance figure that the transmission electron microscope (TEM) of the product of embodiments of the invention 3 obtains.
Fig. 4 is the shape appearance figure that the transmission electron microscope (TEM) of the product of embodiments of the invention 4 obtains.
Fig. 5 is the structure iron that the X-ray powder diffraction (XRD) of the product of embodiments of the invention 1 obtains.
Fig. 6 is the fluorescence emission spectrogram of the product of embodiments of the invention 1.
Embodiment
Further specify the present invention below by embodiment.
Embodiment 1
(1) takes by weighing 0.0025 mole of CaCl respectively
2And Na
2SO
4, then it is dissolved in respectively in 25 ml distilled waters, make the CaCl that volumetric molar concentration is respectively 0.10 mol
2And Na
2SO
4Solution;
(2) in Erlenmeyer flask, add any solution of preparing in 1.5 milliliters of steps (1), 5 milliliters of C in order successively
12E
91 milliliter of Pentyl alcohol and 40 milliliters of hexanaphthenes stirred 5 minutes, formed the reversed phase micelle A solution of transparent homogeneous, and another solution in the step (1) is prepared into another reversed phase micelle B solution with identical method;
(3) two kinds of reversed phase micelle solution with gained in the step (2) mix, stir made its thorough mixing in 2 minutes after, after the standing and reacting 1 minute, reversed phase micelle solution is separated with the acetone breakdown of emulsion, the acetone add-on is 5 milliliters, with product washing each three times,, can obtain product of the present invention with dehydrated alcohol and distilled water 60 ℃ of following vacuum-drying half an hour.
Products therefrom in the step (3) is stored in the dehydrated alcohol, use transmission electron microscope (TEM) and x-ray powder diffraction instrument (XRD) that the pattern and the structure of product are characterized respectively, as can be seen from Fig. 1, product is the nanoparticle of mean diameter 15 nanometers, as can be seen from Fig. 5, XRD result shows product pure (consistent with the JCPDS card).As can be seen from Fig. 6, product has photoluminescence performance.
Embodiment 2
(1) takes by weighing 0.0025 mole of CaCl respectively
2And Na
2SO
4, then it is dissolved in respectively in 25 ml waters, make the CaCl that volumetric molar concentration is respectively 0.10 mol
2And Na
2SO
4Solution;
(2) A: in Erlenmeyer flask, add 1.5 milliliters of CaCl that are mixed with in the step (1) respectively
2Solution, 5 milliliters of C
12E
9, 1 milliliter of Pentyl alcohol and 40 milliliters of hexanaphthenes, stir, form the reversed phase micelle solution of transparent homogeneous;
B: add 1.5 milliliters of Na that are mixed with in the step (1) respectively to Erlenmeyer flask
2SO
4Solution, 5 milliliters of C
12E
9, 1 milliliter of Pentyl alcohol and 40 milliliters of hexanaphthenes, stir, form the another kind of reversed phase micelle solution of transparent homogeneous;
(3) with the two kinds of reversed phase micelle solution stirring of A, B of gained in the step (2), it is mixed, standing and reacting 5 minutes, reversed phase micelle solution is separated with the acetone breakdown of emulsion, the acetone add-on is 6 milliliters, with product washing each three times, 50 ℃ of following vacuum-dryings 60 minutes, the product that obtains was about 50 nanometers of diameter, be about the CaSO of 400 nanometers with dehydrated alcohol and distilled water
4Nanotube, the crystallographic system of product is identical with embodiment 1.The product purity height, degree of crystallinity is good.Compare with embodiment 1, the blue shift degree of fluorescence peak is less.
Embodiment 3
(1) takes by weighing 0.0025 mole of CaCl respectively
2And Na
2SO
4, then it is dissolved in respectively in 25 ml waters, make the CaCl that volumetric molar concentration is respectively 0.10 mol
2And Na
2SO
4Solution;
(2) A: in Erlenmeyer flask, add 1.5 milliliters of CaCl that are mixed with in the step (1) respectively
2Solution, 5 milliliters of C
12E
9, 1 milliliter of Pentyl alcohol and 40 milliliters of hexanaphthenes, stir, form the reversed phase micelle solution of transparent homogeneous;
B: add 1.5 milliliters of Na that are mixed with in the step (1) respectively to Erlenmeyer flask
2SO
4Solution, 5 milliliters of C
12E
9, 1 milliliter of Pentyl alcohol and 40 milliliters of hexanaphthenes, stir, form the another kind of reversed phase micelle solution of transparent homogeneous;
(3) with the two kinds of reversed phase micelle solution stirring of A, B of gained in the step (2), it is mixed, standing and reacting 12 hours, reversed phase micelle solution is separated with the acetone breakdown of emulsion, the acetone add-on is 7 milliliters, with product washing each three times, 70 ℃ of following vacuum-dryings 20 minutes, the product that obtains was about 60 nanometers of diameter, be about 5 microns CaSO with dehydrated alcohol and distilled water
4Nanometer rod, the crystallographic system of product is identical with embodiment 1.The product purity height, degree of crystallinity is better.Compare with embodiment 1, the blue shift degree of fluorescence peak is less.
Embodiment 4
(1) takes by weighing 0.0025 mole of CaCl respectively
2And Na
2SO
4, then it is dissolved in respectively in 25 ml waters, make the CaCl that volumetric molar concentration is respectively 0.10 mol
2And Na
2SO
4Solution;
(2) A: in Erlenmeyer flask, add 1.5 milliliters of CaCl that are mixed with in the step (1) respectively
2Solution, 5 milliliters of C
12E
9, 1 milliliter of Pentyl alcohol and 40 milliliters of hexanaphthenes, stir, form the reversed phase micelle solution of transparent homogeneous;
B: add 1.5 milliliters of Na that are mixed with in the step (1) respectively to Erlenmeyer flask
2SO
4Solution, 5 milliliters of C
12E
9, 1 milliliter of Pentyl alcohol and 40 milliliters of hexanaphthenes, stir, form the another kind of reversed phase micelle solution of transparent homogeneous;
(3) with the two kinds of reversed phase micelle solution stirring of A, B of gained in the step (2), it is mixed, standing and reacting 108 hours, reversed phase micelle solution is separated with the acetone breakdown of emulsion, the acetone add-on is 5 milliliters, with product washing each three times, 70 ℃ of following vacuum-dryings 20 minutes, the product that obtains was about 65 nanometers of diameter, be about 100 microns CaSO with dehydrated alcohol and distilled water
4Nano wire, the crystallographic system of product is identical with embodiment 1.The product purity height, degree of crystallinity is fine.Compare with embodiment 1, the blue shift degree of fluorescence peak is less.
Embodiment 5
(1) takes by weighing 0.0025 mole of CaCl respectively
2And Na
2SO
4, then that it is soluble in water respectively, make the CaCl that volumetric molar concentration is respectively 0.20 mol
2And Na
2SO
4Solution;
(2) A: in Erlenmeyer flask, add 1.5 milliliters of CaCl that are mixed with in the step (1) respectively
2Solution, 5 milliliters of C
12E
9, 1 milliliter of Pentyl alcohol and 40 milliliters of hexanaphthenes, stir, form the reversed phase micelle solution of transparent homogeneous;
B: add 1.5 milliliters of Na that are mixed with in the step (1) respectively to Erlenmeyer flask
2SO
4Solution, 5 milliliters of C
12E
9, 1 milliliter of Pentyl alcohol and 40 milliliters of hexanaphthenes, stir, form the another kind of reversed phase micelle solution of transparent homogeneous;
(3) with the two kinds of reversed phase micelle solution stirring of A, B of gained in the step (2), it is mixed, standing and reacting is in the time of 1.5 minutes, reversed phase micelle solution is separated with the acetone breakdown of emulsion, the acetone add-on is 6 milliliters, with dehydrated alcohol and distilled water product is washed each three times, 60 ℃ of following vacuum-dryings 30 minutes, the product that obtains is the particle of about 20 nanometers of particle diameter, and the crystallographic system of product is identical with embodiment 1.Degree of crystallinity is better.Compare with embodiment 1, the blue shift degree of fluorescence peak diminishes.
Embodiment 6
(1) takes by weighing 0.0025 mole of CaCl respectively
2And K
2SO
4, then it is dissolved in respectively in 25 ml waters, make the CaCl that volumetric molar concentration is respectively 0.10 mol
2And K
2SO
4Solution;
(2) A: in Erlenmeyer flask, add 1.5 milliliters of CaCl that are mixed with in the step (1) respectively
2Solution, 5 milliliters of C
12E
9, 1 milliliter of Pentyl alcohol and 40 milliliters of hexanaphthenes, stir, form the reversed phase micelle solution of transparent homogeneous;
B: add 1.5 milliliters of K that are mixed with in the step (1) respectively to Erlenmeyer flask
2SO
4Solution, 5 milliliters of C
12E
9, 1 milliliter of Pentyl alcohol and 40 milliliters of hexanaphthenes, stir, form the another kind of reversed phase micelle solution of transparent homogeneous;
(3) with the two kinds of reversed phase micelle solution stirring of A, B of gained in the step (2), it is mixed, standing and reacting 12 hours, reversed phase micelle solution is separated with the acetone breakdown of emulsion, the acetone add-on is 5 milliliters, with dehydrated alcohol and distilled water product is washed each three times, 70 ℃ of following vacuum-dryings 20 minutes, the product that obtains is about 63 nanometers of diameter, the CaSO that length is about 6 microns
4Nanometer rod, the crystallographic system of product is identical with embodiment 1.The product purity height, degree of crystallinity and optical property are basic similar to embodiment 1.
Embodiment 7
(1) takes by weighing 0.0025 mole of Ca (NO respectively
3)
2And K
2SO
4, then it is dissolved in respectively in 25 ml waters, make the Ca (NO that volumetric molar concentration is respectively 0.10 mol
3)
2And K
2SO
4Solution;
(2) A: in Erlenmeyer flask, add 1.5 milliliters of Ca (NO that are mixed with in the step (1) respectively
3)
2Solution, 5 milliliters of C
12E
9, 1 milliliter of Pentyl alcohol and 40 milliliters of hexanaphthenes, stir, form the reversed phase micelle solution of transparent homogeneous;
B: add 1.5 milliliters of K that are mixed with in the step (1) respectively to Erlenmeyer flask
2SO
4Solution, 5 milliliters of C
12E
9, 1 milliliter of Pentyl alcohol and 40 milliliters of hexanaphthenes, stir, form the another kind of reversed phase micelle solution of transparent homogeneous;
(3) with the two kinds of reversed phase micelle solution stirring of A, B of gained in the step (2), it is mixed, standing and reacting 12 hours, reversed phase micelle solution is separated with the acetone breakdown of emulsion, and the acetone add-on is 5 milliliters, with dehydrated alcohol and distilled water product is washed each three times, 60 ℃ of following vacuum-dryings 25 minutes, the product that obtains is about 60 nanometers of diameter, the nanometer rod that length is about 5 microns, and the crystallographic system of product is identical with embodiment 1.The product purity height, degree of crystallinity and optical property are basic similar to embodiment 1.
Embodiment 8
(1) 0.0025 mole of CaCl
2And Na
2SO
4, then it is dissolved in respectively in the distilled water, make the CaCl that volumetric molar concentration is 0.05 mol
2And Na
2SO
4Solution;
(2) A: in Erlenmeyer flask, add 1.5 milliliters of CaCl that are mixed with in the step (1) respectively
2Solution, 5 milliliters of C
12E
9, 1 milliliter of Pentyl alcohol and 40 milliliters of hexanaphthenes, stir, form the reversed phase micelle solution of transparent homogeneous;
B: add 1.5 milliliters of Na that are mixed with in the step (1) respectively to Erlenmeyer flask
2SO
4Solution, 5 milliliters of C
12E
9, 1 milliliter of Pentyl alcohol and 40 milliliters of hexanaphthenes, stir, form the another kind of reversed phase micelle solution of transparent homogeneous;
(3) the two kinds of reversed phase micelle solution of A, B with gained in the step (2) mix, after the standing and reacting 1 minute, reversed phase micelle solution is separated with the acetone breakdown of emulsion, the acetone add-on is 5 milliliters, with dehydrated alcohol and distilled water product is washed each three times, 60 ℃ of following vacuum-drying half an hour, the product diameter that obtains is the nanoparticle of 10 nanometers.
Embodiment 9
(1) takes by weighing 0.0025 mole of Ca (NO respectively
3)
2And Na
2SO
4, then that it is soluble in water respectively, make the Ca (NO that volumetric molar concentration is respectively 0.08 mol
3)
2And Na
2SO
4Solution;
(2) A: in Erlenmeyer flask, add 1.5 milliliters of Ca (NO that are mixed with in the step (1) respectively
3)
2Solution, 5 milliliters of C
12E
9, 1 milliliter of Pentyl alcohol and 40 milliliters of hexanaphthenes, stir, form the reversed phase micelle solution of transparent homogeneous;
B: add 1.5 milliliters of Na that are mixed with in the step (1) respectively to Erlenmeyer flask
2SO
4Solution, 5 milliliters of C
12E
9, 1 milliliter of Pentyl alcohol and 40 milliliters of hexanaphthenes, stir, form the another kind of reversed phase micelle solution of transparent homogeneous;
(3) with the two kinds of reversed phase micelle solution stirring of A, B of gained in the step (2), it is mixed, standing and reacting 5.5 minutes, reversed phase micelle solution is separated with the acetone breakdown of emulsion, the acetone add-on is 5 milliliters, with product washing each three times, 50 ℃ of following vacuum-dryings 60 minutes, the product that obtains was about 50 nanometers of diameter, be about the CaSO of 400 nanometers with dehydrated alcohol and distilled water
4Nanotube, the crystallographic system of product is identical with embodiment 1.The product purity height, degree of crystallinity is good.Compare with embodiment 1, the blue shift degree of fluorescence peak is less.
Embodiment 10
(1) takes by weighing 0.0025 mole of CaCl respectively
2And K
2SO
4, then that it is soluble in water respectively, make the CaCl that volumetric molar concentration is respectively 0.15 mol
2And K
2SO
4Solution;
(2) A: in Erlenmeyer flask, add 1.5 milliliters of CaCl that are mixed with in the step (1) respectively
2Solution, 5 milliliters of C
12E
9, 1 milliliter of Pentyl alcohol and 40 milliliters of hexanaphthenes, stir, form the reversed phase micelle solution of transparent homogeneous;
B: add 1.5 milliliters of K that are mixed with in the step (1) respectively to Erlenmeyer flask
2SO
4Solution, 5 milliliters of C
12E
9, 1 milliliter of Pentyl alcohol and 40 milliliters of hexanaphthenes, stir, form the another kind of reversed phase micelle solution of transparent homogeneous;
(3) with the two kinds of reversed phase micelle solution stirring of A, B of gained in the step (2), it is mixed, standing and reacting 15 hours, reversed phase micelle solution is separated with the acetone breakdown of emulsion, the acetone add-on is 5 milliliters, with product washing each three times, 65 ℃ of following vacuum-dryings 25 minutes, the product that obtains was about 65 nanometers of diameter, be about 6.5 microns CaSO with dehydrated alcohol and distilled water
4Nanometer rod, the crystallographic system of product is identical with embodiment 1.The product purity height, degree of crystallinity is better.Compare with embodiment 1, the blue shift degree of fluorescence peak is less.
Embodiment 11
(1) takes by weighing 0.0025 mole of Ca (NO respectively
3)
2And Na
2SO
4, then it is dissolved in respectively in 25 ml waters, make the Ca (NO that volumetric molar concentration is respectively 0.15 mol
3)
2And Na
2SO
4Solution;
(2) A: in Erlenmeyer flask, add 1.5 milliliters of Ca (NO that are mixed with in the step (1) respectively
3)
2Solution, 5 milliliters of C
12E
9, 1 milliliter of Pentyl alcohol and 40 milliliters of hexanaphthenes, stir, form the reversed phase micelle solution of transparent homogeneous;
B: add 1.5 milliliters of Na that are mixed with in the step (1) respectively to Erlenmeyer flask
2SO
4Solution, 5 milliliters of C
12E
9, 1 milliliter of Pentyl alcohol and 40 milliliters of hexanaphthenes, stir, form the another kind of reversed phase micelle solution of transparent homogeneous;
(3) with the two kinds of reversed phase micelle solution stirring of A, B of gained in the step (2), it is mixed, standing and reacting 120 hours, reversed phase micelle solution is separated with the acetone breakdown of emulsion, the acetone add-on is 5 milliliters, with product washing each three times, 65 ℃ of following vacuum-dryings 40 minutes, the product that obtains was about 67 nanometers of diameter, be about 105 microns CaSO with dehydrated alcohol and distilled water
4Nano wire, the crystallographic system of product is identical with embodiment 1.The product purity height, degree of crystallinity is fine.Compare with embodiment 1, the blue shift degree of fluorescence peak is less.
Claims (11)
1, a kind of preparation method of calcium sulfate nanometer material is characterized in that concrete steps are as follows:
(1) take by weighing soluble calcium salt and vitriol, with its solution that is mixed with soluble in water respectively, wherein the mol ratio of calcium salt and vitriol is 1: 1 then, and the calcium salt soln of preparation and sulfate liquor volumetric molar concentration are respectively 0.05～0.20 mol;
(2) A: in Erlenmeyer flask, add 1.5 milliliters of calcium salt solns that are mixed with in the step (1), 5 milliliters of C12E9,1 milliliter of Pentyl alcohol and 40 milliliters of hexanaphthenes respectively, stir, form the reversed phase micelle solution of transparent homogeneous;
B: add 1.5 milliliters of sulfate liquors that are mixed with in the step (1), 5 milliliters of C12E9,1 milliliter of Pentyl alcohol and 40 milliliters of hexanaphthenes respectively to Erlenmeyer flask, stir, form the another kind of reversed phase micelle solution of transparent homogeneous;
(3) the two kinds of reversed phase micelle solution of A, B with gained in the step (2) mix, standing and reacting, and separation, washing, drying promptly obtain required nano material.
2, the preparation method of calcium sulfate nanometer material according to claim 1 is characterized in that described calcium salt is CaCl
2Or Ca (NO
3)
2
3, the preparation method of calcium sulfate nanometer material according to claim 1 is characterized in that described vitriol is Na
2SO
4Or K
2SO
4
4, the preparation method of calcium sulfate nanometer material according to claim 1 is characterized in that the standing and reacting time is 0.8-1.5 minute, obtains the nanoparticle that diameter is the 15-20 nanometer.
5, the preparation method of calcium sulfate nanometer material according to claim 1 is characterized in that the standing and reacting time is 4.5-5.5 minute, obtains the nanotube of 50 nanometers * 400 nanometers.
6, the preparation method of calcium sulfate nanometer material according to claim 1 is characterized in that the standing and reacting time is 10-15 hour, obtains the nanometer rod of 60 nanometers * 5000 nanometers.
7, the preparation method of calcium sulfate nanometer material according to claim 1 is characterized in that the standing and reacting time is 100-120 hour, obtains the nano wire of 65 nanometers * 100000 nanometers.
8, the preparation method of calcium sulfate nanometer material according to claim 1, its feature separate used emulsion splitter in step (3) be acetone, and its add-on is to add the 5-10 milliliter in per 100 ml solns.
9, the preparation method of calcium sulfate nanometer material according to claim 1, its feature adopts dehydrated alcohol and distilled water alternately to clean 3-6 time in described washing.
10, the preparation method of calcium sulfate nanometer material according to claim 1 is characterized in that the dry vacuum-drying of adopting, and temperature is 50-70 ℃, and the time is 20-60 minute.
11, the preparation method of calcium sulfate nanometer material according to claim 1 is characterized in that the gained calcium sulfate nanometer material characterizes by transmission electron microscope or x-ray powder diffraction instrument.
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| CN101550585B (en) * | 2009-04-16 | 2011-10-05 | 北京矿冶研究总院 | Preparation method of dehydrated calcium sulfate whisker |
| CN103754920A (en) * | 2014-01-22 | 2014-04-30 | 瓮福（集团）有限责任公司 | Method for preparing nanometer calcium sulfate |
| CN103922379A (en) * | 2014-03-31 | 2014-07-16 | 北京工业大学 | Preparation method of bunch-shaped calcium sulphate dihydrate |
| CN103964484A (en) * | 2014-05-27 | 2014-08-06 | 湖南恒光科技股份有限公司 | Preparation process of nano anhydrous calcium sulfate |
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2006
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101550585B (en) * | 2009-04-16 | 2011-10-05 | 北京矿冶研究总院 | Preparation method of dehydrated calcium sulfate whisker |
| CN103754920A (en) * | 2014-01-22 | 2014-04-30 | 瓮福（集团）有限责任公司 | Method for preparing nanometer calcium sulfate |
| CN103922379A (en) * | 2014-03-31 | 2014-07-16 | 北京工业大学 | Preparation method of bunch-shaped calcium sulphate dihydrate |
| CN103922379B (en) * | 2014-03-31 | 2015-08-12 | 北京工业大学 | A kind of bouquet shape terra alba preparation method |
| CN103964484A (en) * | 2014-05-27 | 2014-08-06 | 湖南恒光科技股份有限公司 | Preparation process of nano anhydrous calcium sulfate |
| CN103964484B (en) * | 2014-05-27 | 2015-04-01 | 湖南恒光科技股份有限公司 | Preparation process of nano anhydrous calcium sulfate |
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