CN108751247B - Preparation method of nano yttrium oxide with stable BET - Google Patents
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Abstract
The invention belongs to the technical field of preparation of rare earth compounds, and particularly relates to a method for preparing nano yttrium oxide with stable BET (surface area index)A preparation method. The obtained nanometer oxide has primary particle diameter of 30-70nm, uniform particle distribution, and stable specific surface energy in one region of 16-18m2G or 20-22m2(ii) in terms of/g. The method has the advantages of simple process conditions, low production cost and easy realization of industrial production, and the whole preparation process meets the environmental protection requirement.
Description
Technical Field
The present invention belongs to the field of RE oxide preparing technology. In particular to a preparation method of nanometer yttrium oxide with stable BET.
Background
The yttrium oxide is an important rare earth oxide, and the nano powder has good optical, electrical, magnetic, mechanical and chemical properties, and is widely applied to the fields of functional ceramic materials, luminescent materials, laser materials and the like. In the prior art, a chemical precipitation method is adopted to prepare nano yttrium oxide powder, a precipitator is added into an yttrium salt solution to enable anions in the yttrium salt solution to form precipitates, and then the nano yttrium oxide powder is prepared by filtering, washing, drying, thermal decomposition and the like.
However, in the prior art, the concentration of a reaction system is easily uneven by titrating a precipitator into an yttrium salt solution, the growth rate of yttrium ions is difficult to control, and the prepared yttrium oxide powder has large particle size and wide particle size distribution.
The nanometer yttrium oxide powder with higher purity, higher specific surface area, smaller particle size and narrower particle size distribution is a key factor for preparing yttrium aluminum garnet transparent ceramics, yttrium oxide transparent ceramics, gadolinium oxide yttrium transparent ceramics and other transparent ceramics with excellent performance. When the nano yttrium oxide is used in the ceramic and electronic industries, the stability of the raw material nano yttrium oxide needs to be ensured, the primary particle size of a product needs to be ensured, and the specific surface area (BET) of the product needs to be ensured so as to ensure the stability of the final product.
Disclosure of Invention
In order to ensure that the specific surface area of the nano yttrium oxide is in a specified range to meet the requirements of the ceramic and electronic industries, the invention provides a preparation method of the nano yttrium oxide with stable BET (BET surface area) to obtain the nano yttrium oxide with the BET surface area of 16-18m2G and 20-22m2The nanometer yttrium oxide per gram can ensure the uniformity of product particles.
The invention provides a preparation method of nanometer yttrium oxide with stable BET, which comprises the following specific preparation processes:
(1) selecting yttrium chloride feed liquid with acidity less than 0.3mol/l, controlling the concentration of the yttrium chloride feed liquid to be 0.2-0.8mol/l, and adding an anionic surfactant into the feed liquid; selecting a precipitator with the solution concentration of 0.4-1.0 mol/l;
wherein, the anionic surfactant can be polyethylene glycol 2000(PEG2000) or polyethylene glycol 20000(PEG20000), the dosage of the anionic surfactant accounts for 2-5% of the mass percent of the yttrium chloride feed liquid, and the precipitant can be alkaline precipitant such as sodium carbonate, sodium hydroxide or sodium bicarbonate.
The control of the concentration of the yttrium chloride feed liquid and the precipitant solution has great influence on the preparation of the nano yttrium oxide particles, the concentration of the yttrium chloride feed liquid and the precipitant solution is controlled within the range of the invention, the particles within the particle size range of the invention can be prepared, the sizes of the prepared nano yttrium oxide particles are ensured to be consistent, but the particles with higher concentration are bigger if the size of the prepared nano yttrium oxide particles exceeds the range.
(2) Dropwise adding the precipitant solution into the yttrium chloride solution at a constant speed by using a diaphragm pump, controlling the pH value of the salt solution to be 6.5-7 after dropwise adding, stirring for 1h to react to obtain yttrium carbonate or yttrium hydroxide precipitate, then aging for 2h, washing by using a plate-and-frame filter press until no precipitate is generated in the waste water after titration by using silver nitrate.
Wherein the molar ratio of yttrium chloride to precipitant is 1:3-1: 4;
the model of the diaphragm pump: GM500/0.5, manufacturer: zhejiang province, high pump industry, science and technology, Inc.;
the washing temperature is 50-60 ℃;
the type of the plate-and-frame filter press is as follows: XMY-810-U, manufacturer: changzhou wujin chemical machinery ltd;
the diaphragm pump can continuously feed, the middle is not interrupted, the dropping process can be ensured to be uniform, and the uniform dropping can control the formed particles to be uniform, so that the particles of the oxide discharged from the same batch can not be greatly reduced, and the BET of the oxide can be controlled.
The pH of the salt solution is controlled during the reaction, if the pH is less than 6.5, the precipitation is not complete, a part of yttrium ions in the salt solution are not precipitated, the influence on the particles is caused, particles with uneven sizes or agglomerated particles are formed, and the yield of the product is reduced.
The particle size of the oxide will also vary with the washing temperature, and the higher the washing temperature, the larger the particle size, but too low the temperature, the poor washing effect of impurities will be obtained, and the control is best within the scope of the invention by experiment.
And (2) washing by using a plate-and-frame filter press, and pumping air by using a vacuum principle of the plate-and-frame filter press through a vacuum pump to form negative pressure in a plate-and-frame filter press cavity, so that the moisture in the viscous filter cake is pumped away as much as possible, the moisture of each batch of yttrium salt is basically consistent and is about 45-50%, and the weight of the filter cake is consistent.
(3) Drying the washed yttrium carbonate or yttrium hydroxide at 90-120 ℃, then loading the dried yttrium carbonate or yttrium hydroxide into a pot, loading 5-6Kg of yttrium carbonate or yttrium hydroxide into each pot, burning at 900 ℃ in 750-; or loading 7-8Kg of yttrium carbonate or yttrium hydroxide in each bowl, burning at 900 ℃ in 750-.
In the precipitation process, equipment is selected, and process parameters are controlled, so that precipitates with consistent particle size and BET are obtained, but the process parameters in the burning process influence the particle size and the specific surface area of a final product, so that the loading amount of yttrium carbonate and the burning temperature and time are controlled, so that the BET size and the particle size of the final product are controlled. Therefore, the weight of the carbonate precipitated by preparing the same amount of oxide before firing must be consistent, so as to ensure that the weight of the carbonate contained in each pot is approximately the same during firing, so as to ensure that the weight of the oxide fired is the same, which is beneficial for controlling the firing, and thus the BET is relatively stable within a range. And the aim of preparing different BET is fulfilled by adjusting the loading amount of each pot.
Has the advantages that:
the method adopts a precipitation method, uses an alkaline precipitator for precipitation, selects an anionic surfactant as an additive, precipitates rare earth ions, ensures uniform and consistent dropping speed by controlling the acidity and concentration of feed liquid and the concentration of a precipitator solution and adopting a diaphragm pump, adopts a plate-and-frame filter pressing and washing method for washing non-rare earth impurities, utilizes the vacuum principle of a plate-and-frame filter press, pumps air by a vacuum pump, forms negative pressure in a plate-and-frame filter pressing cavity, ensures that moisture in a viscous filter cake is pumped as much as possible, achieves the basic consistency of the moisture of each batch of carbonate, thereby controlling the concentration weight of rare earth salt, then burns and screens to prepare the nano yttrium oxide with the primary particle size of 30-70nm, uniform particle distribution and stable BET, and all elements influence each other to finally obtain the nano yttrium oxide with composite requirements.
Drawings
FIG. 1 is a TEM photograph of nano yttrium oxide prepared in example 1;
FIG. 2 is a TEM photograph of nano-yttria prepared in comparative example 3.
Detailed Description
The present invention will be described in detail with reference to examples.
Example 1
(1) Selecting yttrium chloride feed liquid with acidity less than 0.3mol/l, controlling the concentration of the yttrium chloride feed liquid to be 0.4mol/l, adding an anionic surfactant PEG2000 into the feed liquid, and selecting sodium carbonate with solution concentration of 0.4mol/l as a precipitator;
wherein, the anionic surfactant accounts for 2 percent of the feed liquid by mass.
(2) Dropwise adding a precipitator solution into a yttrium chloride feed liquid at a constant speed by using a diaphragm pump, controlling the pH value of the salt solution to be 6.5-7 after dropwise adding, stirring for 1h to perform precipitation reaction to obtain yttrium carbonate, aging for 2h, washing with water until no precipitate is generated by titrating waste water with silver nitrate, wherein the molar ratio of yttrium chloride to precipitator is 1: 3; the washing temperature is about 55 ℃, and the washing equipment comprises: and (4) a plate-and-frame filter press.
(3) And drying the washed material at 100 ℃, then loading the dried material into bowls, loading 5-6Kg of yttrium carbonate into each bowl, burning at 850 ℃, preserving heat for 3 hours, and sieving to obtain the nano rare earth yttrium oxide.
The primary particle size measured by a scanning electron microscope is as follows: 30-70nm, spherical, uniform size, and good dispersibility, and BET measured by Behcet surface area analyzer is 16-18m2/g。
Example 2
(1) Selecting yttrium chloride feed liquid with acidity less than 0.3mol/l, controlling the concentration of the yttrium chloride feed liquid to be 0.6mol/l, adding an anionic surfactant PEG20000 into the feed liquid, and selecting sodium bicarbonate with solution concentration of 0.5mol/l as a precipitator;
wherein, the anionic surfactant accounts for 3 percent of the feed liquid by mass.
(2) Dropwise adding a precipitator solution into a yttrium chloride feed liquid at a constant speed by using a diaphragm pump, controlling the pH value of the salt solution to be 6.5-7 after dropwise adding, stirring for 1h to perform precipitation reaction to obtain yttrium carbonate, aging for 2h, washing with water until no precipitate is generated by titrating waste water with silver nitrate, wherein the molar ratio of yttrium chloride to precipitator is 1: 4; water washing temperature 50 ℃, water washing equipment: and (4) a plate-and-frame filter press.
(3) And drying the washed material at 90 ℃, then loading the dried material into bowls, loading 5-6Kg of yttrium carbonate into each bowl, burning at 800 ℃, preserving heat for 2.5 hours, and sieving to obtain the nano rare earth yttrium oxide.
The primary particle size measured by a scanning electron microscope is as follows: 30-70nm, spherical, uniform size, and good dispersibility, and BET measured by Behcet surface area analyzer is 16-18m2/g。
Example 3
(1) Selecting yttrium chloride feed liquid with acidity less than 0.3mol/l, controlling the concentration of the yttrium chloride feed liquid to be 0.8mol/l, adding an anionic surfactant PEG20000 into the feed liquid, and selecting sodium bicarbonate with solution concentration of 0.8mol/l as a precipitator;
wherein, the anionic surfactant accounts for 3 percent of the feed liquid by mass.
(2) Dropwise adding a precipitator solution into a yttrium chloride feed liquid at a constant speed by using a diaphragm pump, controlling the pH value of the salt solution to be 6.5-7 after dropwise adding, stirring for 1h to perform precipitation reaction to obtain yttrium carbonate, aging for 2h, washing with water until no precipitate is generated by titrating waste water with silver nitrate, wherein the molar ratio of yttrium chloride to precipitator is 1: 4; water washing temperature 50 ℃, water washing equipment: and (4) a plate-and-frame filter press.
(3) And drying the washed material at 90 ℃, then loading the dried material into bowls, loading 5-6Kg of yttrium carbonate into each bowl, burning at 850 ℃, preserving heat for 2 hours, and sieving to obtain the nano rare earth yttrium oxide.
The primary particle size measured by a scanning electron microscope is as follows: 30-70nm, spherical, uniform size, and good dispersibility, and BET measured by Behcet surface area analyzer is 16-18m2/g。
Example 4
(1) Selecting yttrium chloride feed liquid with acidity less than 0.3mol/l, controlling the concentration of the yttrium chloride feed liquid to be 0.7mol/l, adding an anionic surfactant PEG20000 into the feed liquid, and selecting sodium bicarbonate with solution concentration of 1.0mol/l as a precipitator;
wherein, the anionic surfactant accounts for 4 percent of the feed liquid by mass.
(2) Dropwise adding a precipitator solution into a yttrium chloride feed liquid at a constant speed by using a diaphragm pump, controlling the pH value of the salt solution to be 6.5-7 after dropwise adding, stirring for 1h to perform precipitation reaction to obtain yttrium carbonate, aging for 2h, washing with water until no precipitate is generated by titrating waste water with silver nitrate, wherein the molar ratio of yttrium chloride to precipitator is 1: 4; water washing temperature 50 ℃, water washing equipment: and (4) a plate-and-frame filter press.
(3) And drying the washed material at 90 ℃, then loading the dried material into bowls, loading 5-6Kg of yttrium carbonate into each bowl, burning at 800 ℃, preserving heat for 2.5 hours, and sieving to obtain the nano rare earth yttrium oxide.
The primary particle size measured by a scanning electron microscope is as follows: 30-70nm, spherical, uniform size, and good dispersibility, and BET measured by Behcet surface area analyzer is 16-18m2/g。
Example 5
(1) Selecting yttrium chloride feed liquid with acidity less than 0.3mol/l, controlling the concentration of the yttrium chloride feed liquid to be 0.4mol/l, adding an anionic surfactant PEG2000 into the feed liquid, and selecting sodium bicarbonate with solution concentration of 0.4mol/l as a precipitator;
wherein, the anionic surfactant accounts for 2 percent of the feed liquid by mass.
(2) Dropwise adding a precipitator solution into a yttrium chloride feed liquid at a constant speed by using a diaphragm pump, controlling the pH value of the salt solution to be 6.5-7 after dropwise adding, stirring for 1h to perform precipitation reaction to obtain yttrium carbonate, aging for 2h, washing with water until no precipitate is generated by titrating waste water with silver nitrate, wherein the molar ratio of yttrium chloride to precipitator is 1: 4; the water washing temperature is about 50 ℃, and the water washing equipment comprises: and (4) a plate-and-frame filter press.
(3) And drying the washed material at 100 ℃, then loading the dried material into bowls, loading 7-8Kg of yttrium carbonate into each bowl, burning at 850 ℃, preserving heat for 3 hours, and sieving to obtain the nano rare earth yttrium oxide.
Measured by a scanning electron microscopeThe secondary particle size is as follows: 30-70nm, spherical, uniform size, and good dispersibility, and BET measured by Behcet surface area analyzer is 20-22m2/g。
Example 6
(1) Selecting yttrium chloride feed liquid with acidity less than 0.3mol/l, controlling the concentration of the yttrium chloride feed liquid to be 0.6mol/l, adding an anionic surfactant PEG20000 into the feed liquid, and selecting sodium bicarbonate with solution concentration of 0.6mol/l as a precipitator;
wherein, the anionic surfactant accounts for 3 percent of the feed liquid by mass.
(2) Dropwise adding a precipitator solution into a yttrium chloride feed liquid at a constant speed by using a diaphragm pump, controlling the pH value of the salt solution to be 6.5-7 after dropwise adding, stirring for 1h to perform precipitation reaction to obtain yttrium carbonate, aging for 2h, washing with water until no precipitate is generated by titrating waste water with silver nitrate, wherein the molar ratio of yttrium chloride to precipitator is 1: 4; the washing temperature is about 55 ℃, and the washing equipment comprises: and (4) a plate-and-frame filter press.
(3) And drying the washed material at 120 ℃, then loading the dried material into bowls, loading 7-8Kg of yttrium carbonate into each bowl, burning at 800 ℃, preserving heat for 2.5 hours, and sieving to obtain the nano rare earth yttrium oxide.
The primary particle size measured by a scanning electron microscope is as follows: 30-70nm, spherical, uniform size, and good dispersibility, and BET measured by Behcet surface area analyzer is 20-22m2/g。
Comparative example 1
(1) Selecting yttrium chloride feed liquid with acidity less than 0.3mol/l, controlling the concentration of the yttrium chloride feed liquid to be 0.4mol/l, adding PEG2000 into the feed liquid, and selecting sodium carbonate with solution concentration of 0.4mol/l as a precipitator;
wherein, the anionic surfactant accounts for 2 percent of the feed liquid by mass.
(2) Dropwise adding a precipitator solution into a yttrium chloride feed liquid by using a peristaltic pump, controlling the pH value of the salt solution to be 6.5-7 after dropwise adding, stirring for 1h to perform precipitation reaction to obtain yttrium carbonate, aging for 2h, washing with water until no precipitate is generated in the wastewater by using silver nitrate titration, wherein the molar ratio of yttrium chloride to precipitator is 1: 3; washing equipment with the washing temperature of about 55 ℃: and (4) a plate-and-frame filter press.
(3) And drying the washed material at 100 ℃, then loading the dried material into bowls, loading 5-6Kg of yttrium carbonate into each bowl, burning at 850 ℃, preserving heat for 3 hours, and sieving to obtain the nano rare earth yttrium oxide.
The primary particle size measured by a scanning electron microscope is as follows: 50-150nm, spherical, non-uniform in size, not well dispersed, having agglomeration, BET of 13-20m as measured by Behcet's specific surface apparatus2/g。
Comparative example 2
(1) Selecting yttrium chloride feed liquid with acidity less than 0.3mol/l, controlling the concentration of the yttrium chloride feed liquid to be 0.4mol/l, adding PEG2000 into the feed liquid, and selecting sodium carbonate with solution concentration of 0.4mol/l as a precipitator;
wherein, the anionic surfactant accounts for 2 percent of the feed liquid by mass.
(2) Dropwise adding a precipitator solution into a yttrium chloride feed liquid at a constant speed by using a diaphragm pump, controlling the pH value of the salt solution to be 6.5-7 after dropwise adding, stirring for 1h to perform precipitation reaction to obtain yttrium carbonate, aging for 2h, washing with water until no precipitate is generated by titrating waste water with silver nitrate, wherein the molar ratio of yttrium chloride to precipitator is 1: 3; washing equipment with the washing temperature of about 55 ℃: and (5) pumping the filter barrel.
(3) And drying the washed material at 100 ℃, then loading the dried material into bowls, loading 5-6Kg of yttrium carbonate into each bowl, burning at 850 ℃, preserving heat for 3 hours, and sieving to obtain the nano rare earth yttrium oxide.
The primary particle size measured by a scanning electron microscope is as follows: 30-70nm, spherical, uniform size, and good dispersibility, and BET measured by Behcet surface area analyzer is 25-28m2/g。
Comparative example 3
(1) Selecting yttrium chloride feed liquid with acidity less than 0.3mol/l, controlling the concentration of the yttrium chloride feed liquid to be 0.4mol/l, adding PEG2000 into the feed liquid, and selecting sodium carbonate with solution concentration of 0.4mol/l as a precipitator;
wherein, the anionic surfactant accounts for 2 percent of the feed liquid by mass.
(2) Dropwise adding a precipitator solution into a yttrium chloride feed liquid by using a peristaltic pump, controlling the pH value of the salt solution to be 6.5-7 after dropwise adding, stirring for 1h to perform precipitation reaction to obtain yttrium carbonate, aging for 2h, washing with water until no precipitate is generated in the wastewater by using silver nitrate titration, wherein the molar ratio of yttrium chloride to precipitator is 1: 3; the washing temperature is about 55 ℃, and the washing equipment comprises: and (5) pumping the filter barrel.
(3) And drying the washed material at 100 ℃, then loading the dried material into bowls, loading 5-6Kg of yttrium carbonate into each bowl, burning at 850 ℃, preserving heat for 3 hours, and sieving to obtain the nano rare earth yttrium oxide.
The primary particle size measured by a scanning electron microscope is as follows: 50-150nm, spherical, non-uniform in size, not well dispersed, having agglomeration, BET of 15-28m as measured by Behcet's specific surface apparatus2/g。
Comparative example 4
(1) Selecting yttrium chloride feed liquid with acidity less than 0.3mol/l, controlling the concentration of the yttrium chloride feed liquid to be 0.9mol/l, adding an anionic surfactant PEG2000 into the feed liquid, and selecting sodium bicarbonate with solution concentration of 0.4mol/l as a precipitator;
wherein, the anionic surfactant accounts for 2 percent of the feed liquid by mass.
(2) Dropwise adding a precipitator solution into a yttrium chloride feed liquid at a constant speed by using a diaphragm pump, controlling the pH value of the salt solution to be 6.5-7 after dropwise adding, stirring for 1h to perform precipitation reaction to obtain yttrium carbonate, aging for 2h, washing with water until no precipitate is generated by titrating waste water with silver nitrate, wherein the molar ratio of yttrium chloride to precipitator is 1: 3; the washing temperature is about 55 ℃, and the washing equipment comprises: and (4) a plate-and-frame filter press.
(3) And drying the washed material at 100 ℃, then loading into bowls, loading 5-6Kg of yttrium carbonate into each bowl, burning at 850 ℃, preserving heat for 3 hours, and sieving to obtain the nano rare earth yttrium oxide.
The primary particle size measured by a scanning electron microscope is as follows: 50-100nm, spherical, uniform in size, and good in dispersion, and BET measured by Behcet surface area analyzer is 13-15m2/g。
Comparative example 5
(1) Selecting yttrium chloride feed liquid with acidity less than 0.3mol/l, controlling the concentration of the yttrium chloride feed liquid to be 0.4mol/l, adding an anionic surfactant PEG2000 into the feed liquid, and selecting sodium bicarbonate with solution concentration of 1.2mol/l as a precipitator;
wherein, the anionic surfactant accounts for 2 percent of the feed liquid by mass.
(2) Dropwise adding a precipitator solution into a yttrium chloride feed liquid at a constant speed by using a diaphragm pump, controlling the pH value of the salt solution to be 6.5-7 after dropwise adding, stirring for 1h to perform precipitation reaction to obtain yttrium carbonate, aging for 2h, washing with water until no precipitate is generated by titrating waste water with silver nitrate, wherein the molar ratio of yttrium chloride to precipitator is 1: 3; the washing temperature is about 55 ℃, and the washing equipment comprises: and (4) a plate-and-frame filter press.
(3) And drying the washed material at 100 ℃, then loading 5-6Kg of yttrium carbonate into each bowl, burning at 850 ℃, preserving heat for 3 hours, and sieving to obtain the nano rare earth yttrium oxide.
The primary particle size measured by a scanning electron microscope is as follows: 80-120nm, spherical, uniform size, and good dispersibility, and BET measured by Behcet surface area analyzer is 10-12m2/g。
Claims (5)
1. A preparation method of nanometer yttrium oxide with stable BET is characterized by comprising the following specific processes:
(1) selecting yttrium chloride feed liquid with acidity less than 0.3mol/l, controlling the concentration of the yttrium chloride feed liquid to be 0.2-0.8mol/l, and adding an anionic surfactant into the feed liquid; selecting a precipitator with the solution concentration of 0.4-1.0 mol/l; the precipitant is sodium carbonate, sodium hydroxide or sodium bicarbonate alkaline precipitant;
(2) under the condition of room temperature, dropwise adding a precipitator solution into yttrium chloride feed liquid at a constant speed by using a diaphragm pump, controlling the pH of the salt solution to be 6.5-7 after dropwise adding, stirring for 1h to perform precipitation reaction to obtain yttrium carbonate or yttrium hydroxide, aging for 2h, and then washing by using a plate-and-frame filter press, wherein the washing temperature is as follows: washing at 50-55 deg.C until no precipitate is formed in the wastewater by titration with silver nitrate;
(3) drying the washed yttrium carbonate or yttrium hydroxide at 90-120 ℃, loading into bowls, loading 5-6Kg of yttrium carbonate or yttrium hydroxide into each bowl, firing, preserving heat and sieving to obtain the nano rare earth yttrium oxide; or loading 7-8Kg of yttrium carbonate or yttrium hydroxide in each pot, burning, keeping the temperature, and sieving to obtain the nanometer rare earth yttrium oxide.
2. The method for preparing nano yttrium oxide with stable BET of claim 1, wherein the anionic surfactant is PEG2000 or PEG20000, and the amount of the anionic surfactant is 2-5% by mass of yttrium chloride solution.
3. The method of claim 1, wherein the molar ratio of yttrium chloride to precipitant is in the range of 1:3 to 1: 4.
4. The method for preparing nano yttrium oxide with stable BET of claim 1, wherein the burning temperature is 750-900 ℃ and the holding time is 1-3 hours.
5. A nano yttrium oxide having a stable BET prepared according to the method of claim 1, wherein said prepared nano yttrium oxide has a BET of 16-18m2G or 20-22m2/g。
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CN115959698B (en) * | 2022-12-28 | 2024-05-07 | 广西国盛稀土新材料有限公司 | Method for producing large-particle high-specific gravity yttrium oxide by continuous precipitation |
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