CN112408460B - Preparation method of nano zinc oxide - Google Patents
Preparation method of nano zinc oxide Download PDFInfo
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- CN112408460B CN112408460B CN202011434726.8A CN202011434726A CN112408460B CN 112408460 B CN112408460 B CN 112408460B CN 202011434726 A CN202011434726 A CN 202011434726A CN 112408460 B CN112408460 B CN 112408460B
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- C01G9/00—Compounds of zinc
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Abstract
The invention discloses a preparation method of nano zinc oxide, which comprises the following steps: 1) preparing ammonia-ammonium carbonate mixed liquor: ammonia and ammonium carbonate solution were mixed as 1: (2-3) mixing uniformly according to the volume ratio to prepare an ammonia-ammonium carbonate mixed solution, wherein the solubility of the ammonia water is 0.5-1mol/L, and the concentration of the ammonium carbonate solution is 4-5mol/L; 2) slowly adding zinc oxide into the ammonia-ammonium carbonate mixed solution, wherein the mass volume ratio of the zinc oxide to the ammonia-ammonium carbonate mixed solution is 1-2kg/30L, and uniformly stirring; 3) adding zinc powder, wherein the mass ratio of the added zinc oxide to the zinc powder is 1: (3-4), keeping the temperature of the mixed solution at 40-50 ℃, and filtering to obtain filtrate; 4) slowly heating the filtrate, keeping at 80-90 deg.C for 40-60min, and heating to obtain zinc carbonate precipitate; 5) washing, drying and calcining to obtain the nano zinc oxide. The preparation method of the invention can prepare high-quality nano zinc oxide with high yield and good appearance character under the condition of the same level of cost.
Description
Technical Field
The invention belongs to the field of inorganic material preparation, and particularly relates to a preparation method of nano zinc oxide.
Background
The nano zinc oxide is white or yellowish fine powder with the particle size of 1-100 nm, and is a high-end high-function fine inorganic product.
The nano zinc oxide has the advantages of fine crystal grains, large specific surface area, easy dispersion and the like, shows a plurality of special properties such as non-migration property, fluorescence property, piezoelectricity, ultraviolet absorption and scattering capacity and the like, can be used for manufacturing gas sensors, fluorescent bodies, varistors, ultraviolet shielding materials, image recording materials, piezoelectric materials, piezoresistors, high-efficiency catalysts, magnetic materials, plastic films and the like, and can be used for replacing zinc oxide in the direct method and the Arabian method in the industries such as petroleum catalysts, ceramics, enamel, glass, coatings, medicines, chemistry, paper making and the like.
At present, the methods mainly used for preparing the nano zinc oxide include a direct method, an indirect method, an ammonium-ammonia method and an acid method. However, the preparation of zinc oxide by the ammonia-ammonium method has application difficulties, the quality ratio of ammonia to ammonium carbonate affects the quality of zinc carbonate precipitate, and the impurity removal effect is also affected by the ammonia-ammonium method due to impurities in the raw materials, so that the method has the defects of unstable product properties, high cost and the like.
Disclosure of Invention
The invention aims to provide a preparation method of nano-grade zinc oxide, which is used for preparing the nano-grade zinc oxide by taking industrial-grade zinc oxide as a raw material and has the advantages of high yield, less impurities and low cost.
In order to solve the technical problem, the invention provides a preparation method of nano zinc oxide, which comprises the following steps:
1) preparing ammonia-ammonium carbonate mixed liquor: ammonia and ammonium carbonate solution were mixed as 1: (2-3) mixing uniformly according to the volume ratio to prepare an ammonia-ammonium carbonate mixed solution, wherein the solubility of the ammonia water is 0.5-1mol/L, and the concentration of the ammonium carbonate solution is 4-5mol/L;
2) slowly adding zinc oxide into the ammonia-ammonium carbonate mixed solution, wherein the mass volume ratio of the zinc oxide to the ammonia-ammonium carbonate mixed solution is 1-2kg/30L, and uniformly stirring;
3) adding zinc powder, wherein the mass ratio of the added zinc oxide to the zinc powder is 1: (3-4), keeping the temperature of the mixed solution at 40-50 ℃, and filtering to obtain filtrate;
4) slowly heating the filtrate, keeping at 80-90 deg.C for 40-60min, and heating until zinc carbonate precipitate is obtained;
5) washing, drying and calcining to obtain the nano zinc oxide.
Preferably, the adding speed of the zinc oxide in the step 2) is 200-300 g/min.
Preferably, after the zinc oxide is added in the step 2), the temperature is raised to 40 ℃ and kept for 10 min.
Preferably, the step 4) is specifically: heating at a temperature of 4-7 deg.C/min for 40-60min at 80-90 deg.C, and heating until the mixed solution is boiled to obtain zinc carbonate precipitate.
Preferably, the drying temperature is 60-70 ℃ and the drying time is 2-3 hours.
Preferably, the calcination condition is 550-600 ℃, and the calcination time is 2-3 hours.
Preferably, the adding speed of the zinc powder in the step 3) is 200-300 g/min.
Preferably, the solubility of the ammonia water is 0.6-0.8mol/L, and the concentration of the ammonium carbonate solution is 4.5-5 mol/L.
Preferably, the rate of adding zinc oxide in the step 2) is 250 g/min.
Preferably, the zinc oxide is technical grade zinc oxide.
Compared with the prior art, the preparation method of the nano zinc oxide adopts the ammonia-ammonium method, improves the quality of zinc carbonate precipitation by strictly controlling the concentration of ammonia and ammonium in the solution, and prepares the nano zinc oxide with higher quality by strictly controlling the adding speed of zinc oxide and zinc powder under the condition of the same level of cost, and has less impurities, high yield and good appearance character.
Detailed Description
The core of the invention is to provide a preparation method of nano zinc oxide. The present invention will be described in further detail with reference to specific embodiments in order to make the technical field of the present invention better understood.
Description of the raw materials
Industrial grade zinc oxide: canada brand, Kyowa, Inc.;
zinc powder: the Hunan Fuhao New Material science and technology, Inc., flaky zinc powder.
Example 1
The preparation method of the nano zinc oxide comprises the following steps:
1) preparing ammonia-ammonium carbonate mixed liquor: ammonia and ammonium carbonate solution were mixed as 1: 2 to obtain ammonia-ammonium carbonate mixed solution, wherein the solubility of the ammonia water is 0.5mol/L, and the concentration of the ammonium carbonate solution is 5mol/L;
2) slowly adding zinc oxide into the ammonia-ammonium carbonate mixed solution, wherein the adding speed of the zinc oxide is 200g/min, the mass-volume ratio of the zinc oxide to the ammonia-ammonium carbonate mixed solution is 1kg/30L, uniformly stirring, heating to 40 ℃, and keeping for 10min;
3) adding zinc powder, wherein the adding speed of the zinc powder is 300g/min, and the mass ratio of the added zinc oxide to the zinc powder is 1: 3, keeping the temperature of the mixture at 40-50 ℃, and filtering to obtain filtrate;
4) slowly heating the filtrate to raise the temperature at the speed of 4 ℃/mi, keeping n at 80-90 ℃ for 60min, and then continuously heating until zinc carbonate precipitate is obtained;
5) washing with water;
and (3) drying: the drying temperature is 60-70 ℃, and the drying time is 2-3 hours;
and (3) calcining: the calcining condition is 550-600 ℃, and the calcining time is 2-3 hours;
obtaining the nano zinc oxide.
Example 2
1) Preparing ammonia-ammonium carbonate mixed liquor: ammonia and ammonium carbonate solution were mixed as 1: 3 to obtain ammonia-ammonium carbonate mixed solution, wherein the solubility of the ammonia water is 1mol/L, and the concentration of the ammonium carbonate solution is 4mol/L;
2) slowly adding zinc oxide into the ammonia-ammonium carbonate mixed solution, wherein the adding speed of the zinc oxide is 300g/min, the mass-volume ratio of the zinc oxide to the ammonia-ammonium carbonate mixed solution is 2kg/30L, uniformly stirring, heating to 40 ℃, and keeping for 10min;
3) adding zinc powder, wherein the adding speed of the zinc powder is 200g/min, and the mass ratio of the added zinc oxide to the zinc powder is 1: 4, keeping the temperature of the mixed solution at 40-50 ℃, and filtering to obtain filtrate;
4) slowly heating the filtrate at the temperature rise speed of 7 ℃/mi, keeping n at the temperature of 80-90 ℃ for 40min, and then continuously heating until zinc carbonate precipitate is obtained;
5) washing with water;
and (3) drying: the drying temperature is 60-70 ℃, and the drying time is 2-3 hours;
and (3) calcining: the calcining condition is 550-600 ℃, and the calcining time is 2-3 hours;
obtaining the nano zinc oxide.
Example 3
1) Preparing ammonia-ammonium carbonate mixed liquor: ammonia and ammonium carbonate solution were mixed as 1: 2.5, and uniformly mixing to obtain an ammonia-ammonium carbonate mixed solution, wherein the solubility of the ammonia water is 1mol/L, and the concentration of the ammonium carbonate solution is 4.5mol/L;
2) slowly adding zinc oxide into the ammonia-ammonium carbonate mixed solution at the adding speed of 200g/min, wherein the mass-volume ratio of the zinc oxide to the ammonia-ammonium carbonate mixed solution is 2kg/30L, uniformly stirring, heating to 40 ℃, and keeping for 10min;
3) adding zinc powder, wherein the adding speed of the zinc powder is 200g/min, and the mass ratio of the added zinc oxide to the zinc powder is 1: 4, keeping the temperature of the mixed solution at 40-50 ℃, and filtering to obtain filtrate;
4) slowly heating the filtrate at the temperature rise speed of 5 ℃/mi, keeping n at the temperature of 80-90 ℃ for 40-60min, and then continuously heating until zinc carbonate precipitate is obtained;
5) washing with water;
and (3) drying: the drying temperature is 60-70 ℃, and the drying time is 2-3 hours;
and (3) calcining: the calcining condition is 550-600 ℃, and the calcining time is 2-3 hours;
obtaining the nano zinc oxide.
Comparative example 1
1) Preparing ammonia-ammonium carbonate mixed liquor: ammonia and ammonium carbonate solution were mixed as 1: 6 to obtain ammonia-ammonium carbonate mixed solution, wherein the solubility of the ammonia water is 1mol/L, and the concentration of the ammonium carbonate solution is 8mol/L;
2) slowly adding zinc oxide into the ammonia-ammonium carbonate mixed solution at the adding speed of 200g/min, wherein the mass-volume ratio of the zinc oxide to the ammonia-ammonium carbonate mixed solution is 2kg/30L, uniformly stirring, heating to 40 ℃, and keeping for 10min;
3) adding zinc powder, wherein the adding speed of the zinc powder is 200g/min, and the mass ratio of the added zinc oxide to the zinc powder is 1: 4, keeping the temperature of the mixed solution at 40-50 ℃, and filtering to obtain filtrate;
4) slowly heating the filtrate to raise the temperature at the speed of 5 ℃/mi, keeping n at the temperature of 80-90 ℃ for 40-60min, and then continuing heating until zinc carbonate precipitate is obtained;
5) washing with water;
and (3) drying: the drying temperature is 60-70 ℃, and the drying time is 2-3 hours;
and (3) calcining: the calcining condition is 550-600 ℃, and the calcining time is 2-3 hours;
obtaining the nano zinc oxide.
Comparative example 2
1) Preparing ammonia-ammonium carbonate mixed liquor: ammonia and ammonium carbonate solution were mixed as 1: 2.5, and uniformly mixing to obtain an ammonia-ammonium carbonate mixed solution, wherein the solubility of the ammonia water is 1mol/L, and the concentration of the ammonium carbonate solution is 4.5mol/L;
2) slowly adding zinc oxide into the ammonia-ammonium carbonate mixed solution, wherein the adding speed of the zinc oxide is 500g/min, the mass-volume ratio of the zinc oxide to the ammonia-ammonium carbonate mixed solution is 2kg/30L, uniformly stirring, heating to 40 ℃, and keeping for 10min;
3) adding zinc powder, wherein the adding speed of the zinc powder is 200g/min, and the mass ratio of the added zinc oxide to the zinc powder is 1: 4, keeping the temperature of the mixed solution at 40-50 ℃, and filtering to obtain filtrate;
4) slowly heating the filtrate at the temperature rise speed of 5 ℃/mi, keeping n at the temperature of 80-90 ℃ for 40-60min, and then continuously heating until zinc carbonate precipitate is obtained;
5) washing with water;
and (3) drying: the drying temperature is 60-70 ℃, and the drying time is 2-3 hours;
and (3) calcining: the calcining condition is 550-600 ℃, and the calcining time is 2-3 hours;
obtaining the nano zinc oxide.
Comparative example 3
1) Preparing ammonia-ammonium carbonate mixed liquor: ammonia and ammonium carbonate solution were mixed as 1: 2.5, and uniformly mixing to obtain an ammonia-ammonium carbonate mixed solution, wherein the solubility of the ammonia water is 1mol/L, and the concentration of the ammonium carbonate solution is 4.5mol/L;
2) slowly adding zinc oxide into the ammonia-ammonium carbonate mixed solution at the adding speed of 200g/min, wherein the mass-volume ratio of the zinc oxide to the ammonia-ammonium carbonate mixed solution is 2kg/30L, uniformly stirring, heating to 40 ℃, and keeping for 10min;
3) adding zinc powder, wherein the adding speed of the zinc powder is 500g/min, and the mass ratio of the added zinc oxide to the zinc powder is 1: 4, keeping the temperature of the mixed solution at 40-50 ℃, and filtering to obtain filtrate;
4) slowly heating the filtrate to raise the temperature at the speed of 5 ℃/mi, keeping n at the temperature of 80-90 ℃ for 40-60min, and then continuing heating until zinc carbonate precipitate is obtained;
5) washing with water;
and (3) drying: the drying temperature is 60-70 ℃, and the drying time is 2-3 hours;
and (3) calcining: the calcining condition is 550-600 ℃, and the calcining time is 2-3 hours;
obtaining the nano zinc oxide.
According to the national standard GB/T1958-2004, the nano zinc oxide obtained in examples 1-3 and comparative examples 1-3 is detected, and the lead content, copper content and manganese content of the nano zinc oxide obtained in examples 1-3 are reduced by more than 95% relative to the zinc oxide raw material, while the lead content, copper content and manganese content of the nano zinc oxide obtained in examples 1-3 are reduced by 50-60 relative to the zinc oxide raw material. Because the preparation method strictly controls the proportion of the ammonia-ammonium mixed solution and the adding speeds of the zinc oxide and the zinc powder, the prepared nano zinc oxide has less impurities, high yield and good appearance character at the same level of cost.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (8)
1. A preparation method of nano zinc oxide comprises the following steps:
1) preparing ammonia-ammonium carbonate mixed liquor: ammonia and ammonium carbonate solution were mixed as 1: (2-3) uniformly mixing in a volume ratio to prepare ammonia-ammonium carbonate mixed solution, wherein the concentration of the ammonia water is 0.5-1mol/L, and the concentration of the ammonium carbonate solution is 4-5mol/L;
2) slowly adding zinc oxide into the ammonia-ammonium carbonate mixed solution, wherein the mass volume ratio of the zinc oxide to the ammonia-ammonium carbonate mixed solution is 1-2kg/30L, and uniformly stirring;
3) adding zinc powder, wherein the mass ratio of the added zinc oxide to the zinc powder is 1: (3-4), keeping the temperature of the mixed solution at 40-50 ℃, and filtering to obtain filtrate;
4) slowly heating the filtrate, keeping at 80-90 deg.C for 40-60min, and heating to obtain zinc carbonate precipitate;
5) washing, drying and calcining to obtain nano zinc oxide;
the adding speed of the zinc oxide in the step 2) is 200-300 g/min;
the adding speed of the zinc powder in the step 3) is 200-300 g/min.
2. The method for preparing nano zinc oxide according to claim 1, wherein:
after the zinc oxide is added in the step 2), heating to 40 ℃ and keeping for 10 min.
3. The method for preparing nano zinc oxide according to claim 2, wherein:
the step 4) is specifically as follows: heating at a temperature of 4-7 deg.C/min for 40-60min at 80-90 deg.C, and heating until the mixed solution is boiled to obtain zinc carbonate precipitate.
4. The method for preparing nano zinc oxide according to claim 3, wherein:
the drying temperature is 60-70 ℃, and the drying time is 2-3 hours.
5. The method for preparing nano zinc oxide according to claim 4, wherein:
the calcination condition is 550-600 ℃, and the calcination time is 2-3 hours.
6. The method for preparing nano zinc oxide according to claim 5, wherein the method comprises the following steps:
the solubility of the ammonia water is 0.6-0.8mol/L, and the concentration of the ammonium carbonate solution is 4.5-5 mol/L.
7. The method for preparing nano zinc oxide according to claim 6, wherein:
the speed of adding zinc oxide in the step 2) is 250 g/min.
8. The method for preparing nano zinc oxide according to any one of claims 1 to 7, wherein:
the zinc oxide is technical grade zinc oxide.
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