CN102153131B - Preparation method for zinc oxide nano particles - Google Patents
Preparation method for zinc oxide nano particles Download PDFInfo
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- CN102153131B CN102153131B CN 201110130224 CN201110130224A CN102153131B CN 102153131 B CN102153131 B CN 102153131B CN 201110130224 CN201110130224 CN 201110130224 CN 201110130224 A CN201110130224 A CN 201110130224A CN 102153131 B CN102153131 B CN 102153131B
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Abstract
The invention discloses a preparation method for zinc oxide nano particles, relating to the preparation field of inorganic nonmetal nanometer materials. The preparation method includes the steps as follows; firstly preparing zinc source dispersion solution and oxygen source dispersion solution; adding the oxygen source dispersion solution in the zinc source dispersion solution under the condition of 70-80 DEG C and the dropping time of the oxygen source dispersion solution is 90-120 minutes; reacting to generate white precipitates; later, conducting centrifugal separation on reactant to obtain precipitates; washing, centrifugating and drying the obtained precipitates by distilled water, water-ethanol mixed liquor and absolute ethyl alcohol in sequence; and roasting the obtained precipitates for 3-5 hours at the temperature of 350-470 DEG C to obtain the zinc oxide nano particles. The preparation method has low cost, recyclability, simple equipment, simple and easily-controlled operation conditions, no environment pollution, no toxicity and no harm, and is convenient to large-scale production.
Description
Technical field
The present invention relates to the preparation method of inorganic nonmetallic nanometer material, specifically a kind of preparation method of zinc oxide nano-particle.
Background technology
Nano zine oxide is because particle radius is little; Specific surface area is big; Compare with the common zinc oxide material and to have many strange physics, chemical property; Thereby have incomparable property of common zinc oxide material and new purposes, can nano zine oxide be used for fields such as space flight, electronics, metallurgy, chemistry, biology and environmental protection, and have a good application prospect.
In recent years, owing to nano material has the potential using value to receive much concern in fields such as optics, electricity, magnetics and catalysis.And zinc oxide material have the shielding infrared, ultraviolet, germ-resistant function.Gain great popularity in fields such as novel light shutter device, photochemical catalysis, electrocorrosion.Nano-class zinc oxide is different from the physics of body phase material, the focus that chemical property becomes research because of it especially.At present; The preparation method of the oxide-based nanomaterial of relevant zinc mainly contains reverse micelle method, superpolymer template, hydro-thermal-solvent-thermal method, Gibbs film template, sonochemistry method, hydrothermal synthesis method, microwave irradiation, chemical gas-phase method; Induced with laser method etc., shortcomings such as above method synthesis technique is complicated, the condition difficulty or ease are controlled, environmental pollution is serious, narrow in application range, increase manufacturing cost, increasing labour consumption.
Summary of the invention
Technical problem to be solved by this invention provides that a kind of technology is simple, condition is prone to control, the preparation method of with low cost, pollution-free, applied range, the zinc oxide nano-particle that saves production cost.
The present invention is the deficiency that solves the problems of the technologies described above, and the technical scheme that is adopted is: a kind of preparation method of zinc oxide nano-particle, and the particle diameter of zinc oxide nano-particle is 65-85nm, specific surface area is 4.7059 * 10
7/ m-2.3529 * 10
7/ m.
Its preparation method is:
Step 1, get 1.7-25 parts zinc source by weight, the inorganic salt solution of 20-30 parts of concentration >=0.01mol/L joins the zinc source and makes the dissolving of zinc source in the inorganic salt solution, makes zinc source dispersion soln, and is subsequent use;
Step 2, get 1-25 parts carbonate solution by weight, the inorganic salt solution of 15-30 parts of concentration >=0.01mol/L is added to carbonate solution in the inorganic salt solution, mixes, and makes the oxygen source dispersion soln, and is subsequent use;
Step 3, get oxygen source dispersion soln and zinc source dispersion soln respectively, contain 1 mole oxygen source in the oxygen source dispersion soln of being got, contain 1 mole zinc source in the dispersion soln of zinc source; Oxygen source dispersion soln and zinc source dispersion soln are heated to 70-80 ℃ respectively, keep temperature and the oxygen source dispersion soln is added drop-wise in the dispersion soln of zinc source reaction generation white precipitate; It is 90-120 minutes that the oxygen source dispersion soln dropwises the required time; Post reaction mixture is put into whizzer, with 300-500 rev/mins rotating speed centrifugal 10-20 minutes, obtain throw out A and centrifugate A; Again utilize after centrifugate A reclaims, throw out A is subsequent use;
Step 4, get 1 part throw out A, 8-10 parts zero(ppm) water by weight; Utilize zero(ppm) water that throw out A is washed 1-3 times; After put into separating centrifuge, with 500-800 rev/mins rotating speed centrifugal 5-10 minutes, obtain sediment B and centrifugate B; Again utilize after centrifugate B reclaims, sediment B is subsequent use;
Step 5, get 1 part sediment B, 8-10 parts water-ethanol mixed solution by weight; Utilize the water-ethanol mixed solution that sediment B is carried out 1-3 washings; After put into separating centrifuge, with 500-800 rev/mins rotating speed centrifugal 5-10 minutes, obtain throw out C and centrifugate C; Again utilize after centrifugate C reclaims, throw out C is subsequent use;
Step 6, get 1 part throw out C and 8-10 parts absolute ethyl alcohol by weight, utilize ethanol that throw out C is carried out 1-2 washings, after put into separating centrifuge; With 800-1200 rev/mins rotating speed centrifugal 5-10 minutes, obtain sediment D and centrifugate D, after reclaiming, centrifugate D utilizes again; Sediment D is put into drying baker; Drying, back roasting 3-5 hours under 350-470 ℃ of conditions makes product.
Described zinc source is any one in zinc sulfate or the zinc halide.
Described inorganic salt solution is any one in sodium sulfate, vitriolate of tartar, Repone K or the sodium chloride solution.
Described carbonate is any one in yellow soda ash or the salt of wormwood.
Described water-ethanol mixed solution is got 80% water and 20% absolute ethyl alcohol by volume, mixes the mixed solution that makes.
Described inorganic salt, carbonate and absolute ethyl alcohol are analytical pure.
Described specific surface area is the surface-area in the unit volume.
Beneficial effect
The present invention compared with prior art; Select for use inorganic salt such as metabisulfite solution, potassium sulfate solution, sodium halide solution or potassium halide solution as reaction solvent, these reagent all belong to general commercial goods, buy convenient with low cost; Nontoxic; Can be recycled, environment is not polluted, help environment protection.
In reaction system of the present invention,, select metabisulfite solution, potassium sulfate solution, sodium halide solution or potassium halide formulations prepared from solutions dispersion soln for use to zinc source and the oxygen source selected for use; The negative ions of the dispersion soln of selecting for use can be adsorbed in the nucleating surface of title product through electrical function, slows down nuclei growth speed; And can increase the ionic strength of reaction solution, title product can not be existed with colloid or metamict.Therefore, can make the narrow high-quality nano material of particle size distribution range.
The present invention is added to the oxygen source dispersion soln in the dispersion soln of zinc source, can not zinc source dispersion soln be added in the oxygen source dispersion soln, if zinc source dispersion soln is added in the oxygen source dispersion soln, then can't generate zinc oxide nano-particle; This method is promptly saved energy consumption, reduces environmental pollution again, reduces production costs.The nanometer particle size narrow distribution range of zinc oxide of the present invention; Size can be controlled through reaction soln concentration, reaction times and the temperature of reaction of preparation; Reaction times is shorter, dispersion soln concentration is more little, and the particle diameter of the zinc oxide nano-particle that it makes is just more little; Otherwise under the big more condition of the concentration in longer, the dispersion soln of reaction times, the particle diameter of the zinc oxide nano-particle that makes is just big more.
The adding speed of temperature of reaction and solution is most important among the present invention, and is improper like adding speed and temperature selection, then can't guarantee the productive rate and the particle diameter of zinc oxide nano-particle.Need oxygen source dispersion soln and zinc source dispersion soln be heated to 70-80 ℃ among the present invention; Then the oxygen source dispersion soln is added drop-wise in the dispersion soln of zinc source; It is 90-120 minutes that the oxygen source dispersion soln dropwises the required time, and oxygen source can be dissolved in the solution of zinc source fully, increases the productive rate of zinc oxide; Reduce energy consumption, save production cost.Employed in the present invention inorganic salt are analytical pure, can reduce in the production process sedimentary washing, avoid the loss of zinc oxide, reduce the wasting of resources, save production cost.
Can the centrifugate A that reclaim can directly be used for producing as raw material once more in the present invention; The centrifugate B that reclaims can make its volatilize naturally moisture, recycle once more; The centrifugate C that reclaims, centrifugate D can be used for producing through distillatory method recovery ethanol and zero(ppm) water again, thereby reduce production costs, and reduce the wasting of resources, increase economic benefit, and the method that is used to reclaim is simple, convenient, safe easy handling.
The inventive method is simple, and synthesis temperature is low, condition is prone to control, pollution-free, applied range, and equipment used is simply with low cost, and operational condition simply is easy to grasp, and is convenient to scale operation and in the process of preparation, saves the energy simultaneously, reduces production costs.
Embodiment
A kind of preparation method of zinc oxide nano-particle, step is following:
Step 1, get 1.7-25 parts zinc source by weight, the inorganic salt solution of 20-30 parts of concentration >=0.01mol/L joins the zinc source and makes the dissolving of zinc source in the inorganic salt solution, makes zinc source dispersion soln, and is subsequent use;
Step 2, get 1-25 parts carbonate solution by weight, the inorganic salt solution of 15-30 parts of concentration >=0.01mol/L is added to carbonate solution in the inorganic salt solution, mixes, and makes the oxygen source dispersion soln, and is subsequent use;
Step 3, get oxygen source dispersion soln and zinc source dispersion soln respectively, contain 1 mole oxygen source in the oxygen source dispersion soln of being got, contain 1 mole zinc source in the dispersion soln of zinc source; Oxygen source dispersion soln and zinc source dispersion soln are heated to 70-80 ℃ respectively, keep temperature and the oxygen source dispersion soln is added drop-wise in the dispersion soln of zinc source reaction generation white precipitate; It is 90-120 minutes that the oxygen source dispersion soln dropwises the required time; Post reaction mixture is put into whizzer, with 300-500 rev/mins rotating speed centrifugal 10-20 minutes, obtain throw out A and centrifugate A; Again utilize after centrifugate A reclaims, throw out A is subsequent use;
Step 4, get 1 part throw out A, 8-10 parts zero(ppm) water by weight; Utilize zero(ppm) water that throw out A is washed 1-3 times; After put into separating centrifuge, with 500-800 rev/mins rotating speed centrifugal 5-10 minutes, obtain sediment B and centrifugate B; Again utilize after centrifugate B reclaims, sediment B is subsequent use;
Step 5, get 1 part sediment B, 8-10 parts water-ethanol mixed solution by weight; Utilize the water-ethanol mixed solution that sediment B is carried out 1-3 washings; After put into separating centrifuge, with 500-800 rev/mins rotating speed centrifugal 5-10 minutes, obtain throw out C and centrifugate C; Again utilize after centrifugate C reclaims, throw out C is subsequent use;
Step 6, get 1 part throw out C and 8-10 parts absolute ethyl alcohol by weight, utilize ethanol that throw out C is carried out 1-2 washings, after put into separating centrifuge; With 800-1200 rev/mins rotating speed centrifugal 5-10 minutes, obtain sediment D and centrifugate D, after reclaiming, centrifugate D utilizes again; Sediment D is put into drying baker; Drying, back roasting 3-5 hours under 350-470 ℃ of conditions makes product;
Used zinc source is any one in zinc sulfate or the zinc halide;
Used inorganic salt solution is any one in sodium sulfate, vitriolate of tartar, Repone K or the sodium chloride solution;
Used carbonate is any one in yellow soda ash or the salt of wormwood;
Used water-ethanol mixed solution is got 80% water and 20% absolute ethyl alcohol by volume, mixes the mixed solution that makes;
Used inorganic salt, carbonate and absolute ethyl alcohol are analytical pure;
Specific surface area is the surface-area in the unit volume;
The particle diameter of zinc oxide nano-particle is 65-85nm, and specific surface area is 4.7059 * 10
7/ m-2.3529 * 10
7/ m.
Embodiment one
A kind of preparation method of zinc oxide nano-particle comprises the steps:
Step 1, get 1.7 parts zinc sulfate by weight, 20 parts of concentration are the metabisulfite solution of 0.01mol/L, zinc sulfate is joined make the zinc sulfate dissolving in the metabisulfite solution, can not metabisulfite solution be joined in the zinc sulfate, make zinc source dispersion soln, and are subsequent use;
Step 2, get 1 part sodium carbonate solution by weight, 15 parts of concentration are the metabisulfite solution of 0.01mol/L, and sodium carbonate solution is added in the metabisulfite solution, mix, and make the oxygen source dispersion soln, and are subsequent use;
Step 3, get oxygen source dispersion soln and zinc source dispersion soln respectively, contain 1 mole oxygen source in the oxygen source dispersion soln of being got, contain 1 mole zinc source in the dispersion soln of zinc source; Oxygen source dispersion soln and zinc source dispersion soln are heated to 70 ℃ respectively, keep temperature and the oxygen source dispersion soln is added drop-wise in the dispersion soln of zinc source reaction generation white precipitate; It is 90 minutes that the oxygen source dispersion soln dropwises the required time; Post reaction mixture is put into whizzer, with 300 rev/mins rotating speed centrifugal 10 minutes, obtain throw out A and centrifugate A; Again utilize after centrifugate A reclaims, throw out A is subsequent use;
Step 4, get 1 part throw out A, 8 parts zero(ppm) water by weight, utilize zero(ppm) water that throw out A is washed, after put into separating centrifuge; With 500 rev/mins rotating speed centrifugal 5 minutes; Obtain sediment B and centrifugate B, utilize again after centrifugate B reclaims, sediment B is subsequent use;
Step 5, get 1 part sediment B, 8 parts water-ethanol mixed solution by weight; Utilize the water-ethanol mixed solution that sediment B is washed; After put into separating centrifuge, with 500 rev/mins rotating speed centrifugal 5 minutes, obtain throw out C and centrifugate C; Again utilize after centrifugate C reclaims, throw out C is subsequent use;
Step 6, get 1 part throw out C and 8 parts absolute ethyl alcohol by weight, utilize ethanol that throw out C is washed, after put into separating centrifuge; With 800 rev/mins rotating speed centrifugal 5 minutes, obtain sediment D and centrifugate D, after reclaiming, centrifugate D utilizes again; Sediment D is put into drying baker, drying, back roasting 4 hours under 380 ℃ of conditions; Promptly make zinc oxide nano-particle, particle diameter is 65nm, and specific surface area is 4.7059 * 10
7/ m.
Embodiment two
A kind of preparation method of zinc oxide nano-particle comprises the steps:
Step 1, get 5 parts zinc sulfate by weight, 22 parts of concentration are the metabisulfite solution of 0.02mol/L, zinc sulfate is joined make the zinc sulfate dissolving in the metabisulfite solution, can not metabisulfite solution be joined in the zinc sulfate, make zinc source dispersion soln, and are subsequent use;
Step 2, get 5 parts solution of potassium carbonate by weight, 17 parts of concentration are the metabisulfite solution of 0.02mol/L, and solution of potassium carbonate is added in the metabisulfite solution, mix, and make the oxygen source dispersion soln, and are subsequent use;
Step 3, get oxygen source dispersion soln and zinc source dispersion soln respectively, contain 1 mole oxygen source in the oxygen source dispersion soln of being got, contain 1 mole zinc source in the dispersion soln of zinc source; Oxygen source dispersion soln and zinc source dispersion soln are heated to 72 ℃ respectively, keep temperature and the oxygen source dispersion soln is added drop-wise in the dispersion soln of zinc source reaction generation white precipitate; It is 95 minutes that the oxygen source dispersion soln dropwises the required time; Post reaction mixture is put into whizzer, with 300 rev/mins rotating speed centrifugal 12 minutes, obtain throw out A and centrifugate A; Again utilize after centrifugate A reclaims, throw out A is subsequent use;
Step 4, get 1 part throw out A, 8 parts zero(ppm) water by weight, utilize zero(ppm) water that throw out A is washed, after put into separating centrifuge; With 500 rev/mins rotating speed centrifugal 5 minutes; Obtain sediment B and centrifugate B, utilize again after centrifugate B reclaims, sediment B is subsequent use;
Step 5, get 1 part sediment B, 8 parts water-ethanol mixed solution by weight; Utilize the water-ethanol mixed solution that sediment B is washed; After put into separating centrifuge, with 500 rev/mins rotating speed centrifugal 5 minutes, obtain throw out C and centrifugate C; Again utilize after centrifugate C reclaims, throw out C is subsequent use;
Step 6, get 1 part throw out C and 8 parts absolute ethyl alcohol by weight, utilize ethanol that throw out C is washed, after put into separating centrifuge; With 800 rev/mins rotating speed centrifugal 5 minutes, obtain sediment D and centrifugate D, after reclaiming, centrifugate D utilizes again; Sediment D is put into drying baker, drying, back roasting 3.5 hours under 390 ℃ of conditions; Promptly make zinc oxide nano-particle, particle diameter is 69nm, and specific surface area is 2.8986 * 10
7/ m.
Embodiment three
A kind of preparation method of zinc oxide nano-particle comprises the steps:
Step 1, get 10 parts zinc chloride by weight, 24 parts of concentration are the potassium sulfate solution of 0.04mol/L, zinc chloride is joined make the zinc chloride dissolving in the potassium sulfate solution, can not potassium sulfate solution be joined in the zinc chloride, make zinc source dispersion soln, and are subsequent use;
Step 2, get 10 parts sodium carbonate solution by weight, 20 parts of concentration are the potassium sulfate solution of 0.04mol/L, and sodium carbonate solution is added in the potassium sulfate solution, mix, and make the oxygen source dispersion soln, and are subsequent use;
Step 3, get oxygen source dispersion soln and zinc source dispersion soln respectively, contain 1 mole oxygen source in the oxygen source dispersion soln of being got, contain 1 mole zinc source in the dispersion soln of zinc source; Oxygen source dispersion soln and zinc source dispersion soln are heated to 74 ℃ respectively, keep temperature and the oxygen source dispersion soln is added drop-wise in the dispersion soln of zinc source reaction generation white precipitate; It is 100 minutes that the oxygen source dispersion soln dropwises the required time; Post reaction mixture is put into whizzer, with 300 rev/mins rotating speed centrifugal 14 minutes, obtain throw out A and centrifugate A; Again utilize after centrifugate A reclaims, throw out A is subsequent use;
Step 4, get 1 part throw out A, 8 parts zero(ppm) water by weight, utilize zero(ppm) water that throw out A is washed, after put into separating centrifuge; With 600 rev/mins rotating speed centrifugal 6 minutes; Obtain sediment B and centrifugate B, utilize again after centrifugate B reclaims, sediment B is subsequent use;
Step 5, get 1 part sediment B, 9 parts water-ethanol mixed solution by weight; Utilize the water-ethanol mixed solution that sediment B is washed; After put into separating centrifuge, with 600 rev/mins rotating speed centrifugal 6 minutes, obtain throw out C and centrifugate C; Again utilize after centrifugate C reclaims, throw out C is subsequent use;
Step 6, get 1 part throw out C and 9 parts absolute ethyl alcohol by weight, utilize ethanol that throw out C is washed, after put into separating centrifuge; With 900 rev/mins rotating speed centrifugal 6 minutes, obtain sediment D and centrifugate D, after reclaiming, centrifugate D utilizes again; Sediment D is put into drying baker, drying, back roasting 5 hours under 400 ℃ of conditions; Promptly make zinc oxide nano-particle, particle diameter is 2.8571 * 10 for the 70nm specific surface area
7/ m.
Embodiment four
A kind of preparation method of zinc oxide nano-particle comprises the steps:
Step 1, get 15 parts zinc chloride by weight, 22 parts of concentration are the potassium sulfate solution of 0.05mol/L, zinc chloride is joined make the zinc chloride dissolving in the potassium sulfate solution, can not potassium sulfate solution be joined in the zinc chloride, make zinc source dispersion soln, and are subsequent use;
Step 2, get 15 parts solution of potassium carbonate by weight, 25 parts of concentration are the potassium sulfate solution of 0.05mol/L, and solution of potassium carbonate is added in the potassium sulfate solution, mix, and make the oxygen source dispersion soln, and are subsequent use;
Step 3, get oxygen source dispersion soln and zinc source dispersion soln respectively, contain 1 mole oxygen source in the oxygen source dispersion soln of being got, contain 1 mole zinc source in the dispersion soln of zinc source; Oxygen source dispersion soln and zinc source dispersion soln are heated to 76 ℃ respectively, keep temperature and the oxygen source dispersion soln is added drop-wise in the dispersion soln of zinc source reaction generation white precipitate; It is 105 minutes that the oxygen source dispersion soln dropwises the required time; Post reaction mixture is put into whizzer, with 400 rev/mins rotating speed centrifugal 16 minutes, obtain throw out A and centrifugate A; Again utilize after centrifugate A reclaims, throw out A is subsequent use;
Step 4, get 1 part throw out A, 9 parts zero(ppm) water by weight; Utilize zero(ppm) water that throw out A is carried out 2 washings; After put into separating centrifuge, with 600 rev/mins rotating speed centrifugal 7 minutes, obtain sediment B and centrifugate B; Again utilize after centrifugate B reclaims, sediment B is subsequent use;
Step 5, get 1 part sediment B, 9 parts water-ethanol mixed solution by weight; Utilize the water-ethanol mixed solution that sediment B is carried out 2 washings; After put into separating centrifuge, with 600 rev/mins rotating speed centrifugal 7 minutes, obtain throw out C and centrifugate C; Again utilize after centrifugate C reclaims, throw out C is subsequent use;
Step 6, get 1 part throw out C and 9 parts absolute ethyl alcohol by weight, utilize ethanol that throw out C is washed, after put into separating centrifuge; With 900 rev/mins rotating speed centrifugal 7 minutes, obtain sediment D and centrifugate D, after reclaiming, centrifugate D utilizes again; Sediment D is put into drying baker, drying, back roasting 4.5 hours under 410 ℃ of conditions; Promptly make zinc oxide nano-particle, particle diameter is 73nm, and specific surface area is 2.7397 * 10
7/ m.
Embodiment five
A kind of preparation method of zinc oxide nano-particle comprises the steps:
Step 1, get 18 parts zinc fluoride by weight, 27 parts of concentration are the sodium chloride solution of 0.06mol/L, zinc fluoride is joined make the zinc fluoride dissolving in the sodium chloride solution, can not sodium chloride solution be joined in the zinc fluoride, make zinc source dispersion soln, and are subsequent use;
Step 2, get 18 parts sodium carbonate solution by weight, 25 parts of concentration are the sodium chloride solution of 0.06mol/L, and sodium carbonate solution is added in the sodium chloride solution, mix, and make the oxygen source dispersion soln, and are subsequent use;
Step 3, get oxygen source dispersion soln and zinc source dispersion soln respectively, contain 1 mole oxygen source in the oxygen source dispersion soln of being got, contain 1 mole zinc source in the dispersion soln of zinc source; Oxygen source dispersion soln and zinc source dispersion soln are heated to 78 ℃ respectively, keep temperature and the oxygen source dispersion soln is added drop-wise in the dispersion soln of zinc source reaction generation white precipitate; It is 110 minutes that the oxygen source dispersion soln dropwises the required time; Post reaction mixture is put into whizzer, with 400 rev/mins rotating speed centrifugal 18 minutes, obtain throw out A and centrifugate A; Again utilize after centrifugate A reclaims, throw out A is subsequent use;
Step 4, get 1 part throw out A, 9 parts zero(ppm) water by weight; Utilize zero(ppm) water that throw out A is carried out 2 washings; After put into separating centrifuge, with 700 rev/mins rotating speed centrifugal 8 minutes, obtain sediment B and centrifugate B; Again utilize after centrifugate B reclaims, sediment B is subsequent use;
Step 5, get 1 part sediment B, 9 parts water-ethanol mixed solution by weight; Utilize the water-ethanol mixed solution that sediment B is carried out 2 washings; After put into separating centrifuge, with 700 rev/mins rotating speed centrifugal 8 minutes, obtain throw out C and centrifugate C; Again utilize after centrifugate C reclaims, throw out C is subsequent use;
Step 6, get 1 part throw out C and 9 parts absolute ethyl alcohol by weight, utilize ethanol that throw out C is carried out 2 washings, after put into separating centrifuge; With 1000 rev/mins rotating speed centrifugal 8 minutes, obtain sediment D and centrifugate D, after reclaiming, centrifugate D utilizes again; Sediment D is put into drying baker, drying, back roasting 4 hours under 430 ℃ of conditions; Promptly make zinc oxide nano-particle, particle diameter is 75nm, and specific surface area is 2.6667 * 10
7/ m.
Embodiment six
A kind of preparation method of zinc oxide nano-particle comprises the steps:
Step 1, get 20 parts zinc fluoride by weight, 28 parts of concentration are the sodium chloride solution of 0.07mol/L, zinc fluoride is joined make the zinc fluoride dissolving in the sodium chloride solution, can not sodium chloride solution be joined in the zinc fluoride, make zinc source dispersion soln, and are subsequent use;
Step 2, get 20 parts solution of potassium carbonate by weight, 25 parts of concentration are the sodium chloride solution of 0.07mol/L, and solution of potassium carbonate is added in the sodium chloride solution, mix, and make the oxygen source dispersion soln, and are subsequent use;
Step 3, get oxygen source dispersion soln and zinc source dispersion soln respectively, contain 1 mole oxygen source in the oxygen source dispersion soln of being got, contain 1 mole zinc source in the dispersion soln of zinc source; Oxygen source dispersion soln and zinc source dispersion soln are heated to 79 ℃ respectively, keep temperature and the oxygen source dispersion soln is added drop-wise in the dispersion soln of zinc source reaction generation white precipitate; It is 115 minutes that the oxygen source dispersion soln dropwises the required time; Post reaction mixture is put into whizzer, with 500 rev/mins rotating speed centrifugal 19 minutes, obtain throw out A and centrifugate A; Again utilize after centrifugate A reclaims, throw out A is subsequent use;
Step 4, get 1 part throw out A, 10 parts zero(ppm) water by weight; Utilize zero(ppm) water that throw out A is carried out 3 washings; After put into separating centrifuge, with 700 rev/mins rotating speed centrifugal 9 minutes, obtain sediment B and centrifugate B; Again utilize after centrifugate B reclaims, sediment B is subsequent use;
Step 5, get 1 part sediment B, 10 parts water-ethanol mixed solution by weight; Utilize the water-ethanol mixed solution that sediment B is carried out 3 washings; After put into separating centrifuge, with 700 rev/mins rotating speed centrifugal 9 minutes, obtain throw out C and centrifugate C; Again utilize after centrifugate C reclaims, throw out C is subsequent use;
Step 6, get 1 part throw out C and 10 parts absolute ethyl alcohol by weight, utilize ethanol that throw out C is carried out 2 washings, after put into separating centrifuge; With 1100 rev/mins rotating speed centrifugal 9 minutes, obtain sediment D and centrifugate D, after reclaiming, centrifugate D utilizes again; Sediment D is put into drying baker, drying, back roasting 4.5 hours under 440 ℃ of conditions; Promptly make zinc oxide nano-particle, particle diameter is 78nm, and specific surface area is 2.5641 * 10
7/ m.
Embodiment seven
A kind of preparation method of zinc oxide nano-particle comprises the steps:
Step 1, get 22 parts zinc bromide by weight, 29 parts of concentration are the Klorvess Liquid of 0.08mol/L, zinc bromide is joined bromizate the zinc dissolving in the Klorvess Liquid, can not Klorvess Liquid be joined in the zinc bromide, make zinc source dispersion soln, and are subsequent use;
Step 2, get 24 parts sodium carbonate solution by weight, 29 parts of concentration are the Klorvess Liquid of 0.08mol/L, and sodium carbonate solution is added in the Klorvess Liquid, mix, and make the oxygen source dispersion soln, and are subsequent use;
Step 3, get oxygen source dispersion soln and zinc source dispersion soln respectively, contain 1 mole oxygen source in the oxygen source dispersion soln of being got, contain 1 mole zinc source in the dispersion soln of zinc source; Oxygen source dispersion soln and zinc source dispersion soln are heated to 80 ℃ respectively, keep temperature and the oxygen source dispersion soln is added drop-wise in the dispersion soln of zinc source reaction generation white precipitate; It is 115 minutes that the oxygen source dispersion soln dropwises the required time; Post reaction mixture is put into whizzer, with 500 rev/mins rotating speed centrifugal 19 minutes, obtain throw out A and centrifugate A; Again utilize after centrifugate A reclaims, throw out A is subsequent use;
Step 4, get 1 part throw out A, 10 parts zero(ppm) water by weight; Utilize zero(ppm) water that throw out A is carried out 3 washings; After put into separating centrifuge, with 800 rev/mins rotating speed centrifugal 10 minutes, obtain sediment B and centrifugate B; Again utilize after centrifugate B reclaims, sediment B is subsequent use;
Step 5, get 1 part sediment B, 10 parts water-ethanol mixed solution by weight; Utilize the water-ethanol mixed solution that sediment B is carried out 3 washings; After put into separating centrifuge, with 800 rev/mins rotating speed centrifugal 10 minutes, obtain throw out C and centrifugate C; Again utilize after centrifugate C reclaims, throw out C is subsequent use;
Step 6, get 1 part throw out C and 10 parts absolute ethyl alcohol by weight, utilize ethanol that throw out C is carried out 2 washings, after put into separating centrifuge; With 1200 rev/mins rotating speed centrifugal 10 minutes, obtain sediment D and centrifugate D, after reclaiming, centrifugate D utilizes again; Sediment D is put into drying baker, drying, back roasting 3.5 hours under 460 ℃ of conditions; Promptly make zinc oxide nano-particle, particle diameter is 80nm, and specific surface area is 2.4391 * 10
7/ m.
Embodiment eight
A kind of preparation method of zinc oxide nano-particle comprises the steps:
Step 1, get 25 parts zinc bromide by weight, 30 parts of concentration are the Klorvess Liquid of 0.1mol/L, zinc bromide is joined bromizate the zinc dissolving in the Klorvess Liquid, can not Klorvess Liquid be joined in the zinc bromide, make zinc source dispersion soln, and are subsequent use;
Step 2, get 25 parts solution of potassium carbonate by weight, 30 parts of concentration are the Klorvess Liquid of 0.1mol/L, and solution of potassium carbonate is added in the Klorvess Liquid, mix, and make the oxygen source dispersion soln, and are subsequent use;
Step 3, get oxygen source dispersion soln and zinc source dispersion soln respectively, contain 1 mole oxygen source in the oxygen source dispersion soln of being got, contain 1 mole zinc source in the dispersion soln of zinc source; Oxygen source dispersion soln and zinc source dispersion soln are heated to 80 ℃ respectively, keep temperature and the oxygen source dispersion soln is added drop-wise in the dispersion soln of zinc source reaction generation white precipitate; It is 120 minutes that the oxygen source dispersion soln dropwises the required time; Post reaction mixture is put into whizzer, with 500 rev/mins rotating speed centrifugal 20 minutes, obtain throw out A and centrifugate A; Again utilize after centrifugate A reclaims, throw out A is subsequent use;
Step 4, get 1 part throw out A, 10 parts zero(ppm) water by weight; Utilize zero(ppm) water that throw out A is carried out 3 washings; After put into separating centrifuge, with 800 rev/mins rotating speed centrifugal 10 minutes, obtain sediment B and centrifugate B; Again utilize after centrifugate B reclaims, sediment B is subsequent use;
Step 5, get 1 part sediment B, 10 parts water-ethanol mixed solution by weight; Utilize the water-ethanol mixed solution that sediment B is carried out 3 washings; After put into separating centrifuge, with 800 rev/mins rotating speed centrifugal 10 minutes, obtain throw out C and centrifugate C; Again utilize after centrifugate C reclaims, throw out C is subsequent use;
Step 6, get 1 part throw out C and 10 parts absolute ethyl alcohol by weight, utilize ethanol that throw out C is carried out 2 washings, after put into separating centrifuge; With 1200 rev/mins rotating speed centrifugal 10 minutes, obtain sediment D and centrifugate D, after reclaiming, centrifugate D utilizes again; Sediment D is put into drying baker, drying, back roasting 3 hours under 470 ℃ of conditions; Promptly make zinc oxide nano-particle, particle diameter is 85nm, and specific surface area is 2.3529 * 10
7/ m.
Claims (4)
1. the preparation method of a zinc oxide nano-particle, it is characterized in that: the particle diameter of described zinc oxide nano-particle is 65-85nm, specific surface area is 4.7059 * 10
7/ m-2.3529 * 10
7/ m:
Its preparation method is:
Step 1, get 1.7-25 parts zinc source by weight, the inorganic salt solution of 20-30 parts of concentration >=0.01mol/L joins the zinc source and makes the dissolving of zinc source in the inorganic salt solution, makes zinc source dispersion soln, and is subsequent use;
Step 2, get 1-25 parts carbonate solution by weight, the inorganic salt solution of 15-30 parts of concentration >=0.01mol/L is added to carbonate solution in the inorganic salt solution, mixes, and makes the oxygen source dispersion soln, and is subsequent use;
Step 3, get oxygen source dispersion soln and zinc source dispersion soln respectively, contain 1 mole oxygen source in the oxygen source dispersion soln of being got, contain 1 mole zinc source in the dispersion soln of zinc source; Oxygen source dispersion soln and zinc source dispersion soln are heated to 70-80 ℃ respectively, keep temperature and the oxygen source dispersion soln is added drop-wise in the dispersion soln of zinc source reaction generation white precipitate; It is 90-120 minutes that the oxygen source dispersion soln dropwises the required time; Post reaction mixture is put into whizzer, with 300-500 rev/mins rotating speed centrifugal 10-20 minutes, obtain throw out A and centrifugate A; Again utilize after centrifugate A reclaims, throw out A is subsequent use;
Step 4, get 1 part throw out A, 8-10 parts zero(ppm) water by weight; Utilize zero(ppm) water that throw out A is washed 1-3 times; After put into separating centrifuge, with 500-800 rev/mins rotating speed centrifugal 5-10 minutes, obtain sediment B and centrifugate B; Again utilize after centrifugate B reclaims, sediment B is subsequent use;
Step 5, get 1 part sediment B, 8-10 parts water-ethanol mixed solution by weight; Utilize the water-ethanol mixed solution that sediment B is carried out 1-3 washings; After put into separating centrifuge, with 500-800 rev/mins rotating speed centrifugal 5-10 minutes, obtain throw out C and centrifugate C; Again utilize after centrifugate C reclaims, throw out C is subsequent use;
Step 6, get 1 part throw out C and 8-10 parts absolute ethyl alcohol by weight, utilize ethanol that throw out C is carried out 1-2 washings, after put into separating centrifuge; With 800-1200 rev/mins rotating speed centrifugal 5-10 minutes, obtain sediment D and centrifugate D, after reclaiming, centrifugate D utilizes again; Sediment D is put into drying baker; Drying, back roasting 3-5 hours under 350-470 ℃ of conditions makes product;
Described carbonate is any one in yellow soda ash or the salt of wormwood.
2. the preparation method of a kind of zinc oxide nano-particle according to claim 1 is characterized in that described zinc source is any one in zinc sulfate or the zinc halide.
3. the preparation method of a kind of zinc oxide nano-particle according to claim 1 is characterized in that described inorganic salt solution is any one in sodium sulfate, vitriolate of tartar, Repone K or the sodium chloride solution.
4. the preparation method of a kind of zinc oxide nano-particle according to claim 1 is characterized in that described water-ethanol mixed solution gets 80% water and 20% absolute ethyl alcohol by volume, mixes the mixed solution that makes.
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| CN108298502B (en) * | 2018-01-15 | 2021-06-01 | 东南大学 | Method for preparing dispersed nano metal oxide and nano metal powder |
| CN110451555A (en) * | 2019-09-06 | 2019-11-15 | 辽宁星空钠电电池有限公司 | A kind of method that rapid precipitation prepares one-dimensional zinc hydroxide nanometer rods |
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| CN1296041A (en) * | 2000-11-30 | 2001-05-23 | 上海博纳科技发展有限公司 | Process for preparing nanometer zinc oxide |
| CN101823758A (en) * | 2010-05-14 | 2010-09-08 | 常宁市湘江化工有限责任公司 | Novel method for producing nanometer grade zinc carbonate and zinc oxide |
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| CN1296041A (en) * | 2000-11-30 | 2001-05-23 | 上海博纳科技发展有限公司 | Process for preparing nanometer zinc oxide |
| CN101823758A (en) * | 2010-05-14 | 2010-09-08 | 常宁市湘江化工有限责任公司 | Novel method for producing nanometer grade zinc carbonate and zinc oxide |
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| Title |
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| 商连弟等.氧化锌生产方法及研究进展.《无机盐工业》.2008,第40卷(第3期),4-7. * |
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