CN110885095B - Method for preparing porous calcium titanate based on eutectic solvent - Google Patents
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Abstract
The invention relates to a method for preparing porous calcium titanate based on a eutectic solvent, belonging to the field of inorganic nonmetallic materials. The method for preparing the porous calcium titanate comprises the following steps: uniformly mixing a hydrogen bond acceptor and a hydrogen bond donor according to the molar ratio of 1-1.5:1-3 to obtain a eutectic solvent; adding calcium-containing substances and titanium dioxide into a eutectic solvent according to a liquid-solid ratio of 1:4-30, and mixing for 1-5h at 20-60 ℃ to obtain a mixed solution; wherein the molar ratio of the calcium-containing substance to the titanium dioxide is 1: 1; the calcium-containing substance is calcium oxide or calcium hydroxide: mixing the obtained mixed solution with water at a volume ratio of 1:5-20, standing for precipitation, and filtering to obtain solid substance; calcining, controlling the heating rate to be 2-5 ℃/min, heating to 875-950 ℃, calcining for 3-5 h, and cooling to obtain the porous calcium titanate powder. The method of the invention can be carried out at lower temperature.
Description
Technical Field
The invention relates to a method for preparing porous calcium titanate based on a eutectic solvent, belonging to the field of inorganic nonmetallic materials.
Background
Calcium titanate is a typical representative of perovskite type oxides, and its ideal structure is generally cubic or octahedral. As an inorganic non-metallic material, the inorganic non-metallic material has unique structure, good stability, biocompatibility, rich raw materials and low preparation cost, is widely applied to the fields of photocatalysis, dielectric property, optical property, electricity, biological material and the like, has very important significance in the aspects of basic research and practical application, and is very important for basic research and practical application of many disciplines including geology, solid chemistry, material science, electronic engineering, biotechnology and the like. At present, perovskite type oxide has shown a plurality of special properties in the fields of optics, electrics, biology and the like, and has become a research hotspot of functional oxide materials. At present, the conventional methods commonly used for preparing calcium titanate powder are a solid-phase synthesis method and a solvothermal method. The solid-phase synthesis method is controlled by solid-phase diffusion in the reaction, needs higher temperature and long-time reaction, has the defects of large energy consumption, uneven particle size, difficult control of microstructure and the like, and has the problems that the obtained powder product is easy to agglomerate, further processes such as crushing, grinding and the like are needed, impurities are easy to introduce and the like. The solvothermal method is to perform related chemical reactions at high temperature and high pressure, and although the reaction temperature is relatively low, the used solvent is usually an organic solvent and the reaction process usually requires the use of an autoclave, which causes environmental hazards in the production process. Therefore, the method for preparing calcium titanate, which is environment-friendly, simple in process flow and low in cost, is especially important.
At present, calcium titanate materials are generally prepared by taking calcium chloride and titanium oxide as raw materials, and titanium oxide and calcium oxide are rarely used as raw materials to prepare calcium titanate. The reason is that titanium oxide and calcium oxide are directly used as raw materials to prepare calcium titanate, the sintering temperature is higher, about 1450 ℃, so the preparation method has certain requirements on equipment and higher energy consumption (Hanming & cleaning, Zhang, research on synthesis and calcination by sintering method, Liaoning university of science and technology). In the prior art, a method for preparing calcium titanate by taking titanium oxide and calcium oxide as raw materials is also disclosed, wherein the calcium titanate is obtained by fully mixing the calcium oxide, the titanium oxide and other additives, grinding, performing extrusion forming, calcining at 1350 ℃, and crushing and grinding after calcining. In the method, in order to lower the sintering temperature of calcium titanate, additives are added to the raw materials of titanium oxide and calcium oxide, but even if other additives are added, the sintering temperature can be only lowered to 1350 ℃. The sintering temperature is still high.
Disclosure of Invention
The first technical problem to be solved by the invention is to provide a method for preparing porous calcium titanate by taking titanium oxide and calcium oxide as raw materials, wherein the sintering temperature is low.
The method for preparing the porous calcium titanate based on the eutectic solvent comprises the following steps:
a. preparing a eutectic solvent: uniformly mixing a hydrogen bond acceptor and a hydrogen bond donor according to the molar ratio of 1-1.5:1-3 to obtain a eutectic solvent; wherein the hydrogen bond acceptor is a quaternary ammonium salt or betaine; the hydrogen bond donor is a carboxylic acid;
b. dissolving raw materials: adding calcium-containing substances and titanium dioxide into a eutectic solvent according to a liquid-solid ratio of 1:4-30, and mixing for 1-5h at 20-60 ℃ to obtain a mixed solution; wherein the molar ratio of the calcium-containing substance to the titanium dioxide is 1: 1; the calcium-containing substance is calcium oxide or calcium hydroxide;
c. solution dilution and precipitation: uniformly mixing the mixed solution prepared in the step b with water according to the volume ratio of 1:5-20, standing, precipitating and filtering to obtain a solid substance;
d. and (3) calcining: and calcining the solid matter, controlling the heating rate to be 2-5 ℃/min, heating to 875-950 ℃, calcining for 3-5 h, and cooling to room temperature to obtain the porous calcium titanate powder.
Preferably, in step a: the hydrogen bond acceptor is quaternary ammonium salt; more preferably, the quaternary ammonium salt is at least one of choline chloride and benzyltriethylammonium chloride; most preferably, the hydrogen bond acceptor is choline chloride.
Preferably, in step a: the hydrogen bond donor is oxalic acid, malic acid, citric acid or succinic acid; more preferably, the hydrogen bond donor is oxalic acid.
Preferably, in step a: the molar ratio of the hydrogen bond acceptor to the hydrogen bond donor is 1: 1-2; more preferably, the molar ratio of hydrogen bond acceptor to hydrogen bond donor is 1: 2.
Preferably, in step b: the granularity of the calcium-containing substance is less than or equal to 100 meshes, and the granularity of the titanium dioxide is less than or equal to 100 meshes.
Preferably, in step b: the liquid-solid ratio is 1: 10-15; preferably, the liquid-to-solid ratio is 1: 10.
Preferably, in step b: adding the calcium-containing substance and titanium dioxide into the eutectic solvent, and uniformly mixing at 40-60 ℃.
Preferably, in step b: the temperature is 50 ℃, and the mixing time is 1-5 h; more preferably the mixing time is 1-2 h.
Preferably, in step b: mixing is carried out in a stirring mode, and the stirring speed is controlled to be 50-400 rpm; more preferably, the stirring speed is 100-.
Preferably, in the step c, the mixed solution prepared in the step b is uniformly mixed with water according to the volume ratio of 1: 10-20.
Preferably, in step c, the precipitation time is 2-4 h.
Preferably, in step d: heating to 875-925 ℃, and calcining for 4-5 h.
The invention also provides porous calcium titanate.
The porous calcium titanate is prepared by adopting the eutectic solvent.
Compared with the prior art, the invention has the beneficial effects that:
1. the method adopts the eutectic solvent to dissolve calcium oxide and titanium dioxide, adds water to separate out precipitate, and calcines the precipitate to obtain the porous calcium titanate powder.
2. The used eutectic solvent belongs to a green chemical solvent, and compared with ionic liquid such as pyrrole and pyridine, the eutectic solvent has the advantages of simple synthesis and low cost.
3. The porous calcium titanate prepared by the method has high yield which is more than or equal to 99.3 percent.
Drawings
Figure 1 is the XRD pattern of the product of example 1.
FIG. 2 is an SEM image of the product of example 1.
Detailed Description
The first technical problem to be solved by the invention is to provide a method for preparing porous calcium titanate by taking titanium oxide and calcium oxide as raw materials, wherein the sintering temperature is low.
The method for preparing the porous calcium titanate based on the eutectic solvent comprises the following steps:
a. preparing a eutectic solvent: uniformly mixing a hydrogen bond acceptor and a hydrogen bond donor according to the molar ratio of 1-1.5:1-3 to obtain a eutectic solvent; wherein the hydrogen bond acceptor is a quaternary ammonium salt or betaine; the hydrogen bond donor is a carboxylic acid;
b. dissolving raw materials: adding calcium-containing substances and titanium dioxide into a eutectic solvent according to a liquid-solid ratio of 1:4-30, and mixing for 1-5h at 20-60 ℃ to obtain a mixed solution; wherein the molar ratio of the calcium-containing substance to the titanium dioxide is 1: 1; the calcium-containing substance is calcium oxide or calcium hydroxide;
c. solution dilution and precipitation: uniformly mixing the mixed solution prepared in the step b with water according to the volume ratio of 1:5-20, standing, precipitating and filtering to obtain a solid substance;
d. and (3) calcining: and calcining the solid matter, controlling the heating rate to be 2-5 ℃/min, heating to 875-950 ℃, calcining for 3-5 h, and cooling to room temperature to obtain the porous calcium titanate powder.
The eutectic solvent is a eutectic mixture formed by combining compounds such as hydrogen bond donors, hydrogen bond acceptors and the like in a certain stoichiometric ratio. The eutectic solvent used in the method has the advantages of wide electrochemical window, good solubility and conductivity, low vapor pressure, good physical and chemical stability and the like. Compared with the traditional solvent, the solvent has the advantages of low vapor pressure, good solubility, good physical and chemical stability and the like.
According to the method, the eutectic solvent is used as the solvent to prepare the calcium titanate, so that the sintering temperature is reduced, and the porous calcium titanate with controllable morphology and size is prepared. Therefore, the eutectic solvent is used as a solvent to prepare the calcium titanate with controllable shape and size, and has wide application prospect.
If the eutectic solvent is not used, the calcium oxide and the titanium oxide are directly calcined at 875-950 ℃ for 3-5 hours, and the calcium titanate cannot be obtained.
Preferably, in step a: the hydrogen bond acceptor is quaternary ammonium salt; more preferably, the quaternary ammonium salt is at least one of choline chloride and benzyltriethylammonium chloride; most preferably, the hydrogen bond acceptor is choline chloride.
Preferably, in step a: the hydrogen bond donor is oxalic acid, malic acid, citric acid or succinic acid; more preferably, the hydrogen bond donor is oxalic acid.
Preferably, in step a: the molar ratio of the hydrogen bond acceptor to the hydrogen bond donor is 1: 1-2; more preferably, the molar ratio of hydrogen bond acceptor to hydrogen bond donor is 1: 2.
Wherein, in order to improve the purity of the prepared product, the molar ratio of the calcium-containing substance to the titanium dioxide is 1:1.
Preferably, in step b: the granularity of the calcium-containing substance is less than or equal to 100 meshes, and the granularity of the titanium dioxide is less than or equal to 100 meshes.
In the step b, a raw material dissolving step: adding calcium-containing materials and titanium dioxide into a eutectic solvent according to a liquid-solid ratio of 1:4-30, mixing, controlling the temperature to be 20-60 ℃, and dissolving for 1-5 hours. Wherein the liquid-solid ratio is a liquid-solid mass ratio, which is the mass of the eutectic solvent/(the mass of the calcium-containing substance + the mass of the titanium dioxide).
Preferably, in step b: the liquid-solid ratio is 1: 10-15; preferably, the liquid-to-solid ratio is 1: 10.
Wherein, in the step b: the temperature is 50 ℃, and the mixing time is 1-5 h; if the mixing time is too short, the calcium-containing substance is not sufficiently dissolved and is not uniformly mixed with the titanium dioxide. More preferably the mixing time is 1-2 h.
In order to mix the product more uniformly, preferably, in step b: the mixing is carried out in a stirring mode, and the stirring speed is controlled to be 50-400 rpm.
Preferably, in step c, standing for 2-5h, if the time is too short, part of the solid phase has not yet settled; the product yield is affected; the time is too long, and the time for preparing the product is prolonged. Preferably, in step c: the precipitation time is 2-4 h.
In the step d, the calcining temperature is 875-950 ℃, and the calcining time is 3-5 hours; if the calcining temperature is too low, the product can not obtain calcium titanate; too short a calcination time may result in impure product, yet insufficient decomposition. Preferably, in step d: heating to 875-925 ℃, and calcining for 4-5 h.
In the step d, the heating rate is controlled to be 2-5 ℃/min, and the particle size of the powder is larger and the size of the powder is not uniform due to the excessively high heating rate.
Under the calcination conditions of the present invention, calcium titanate having a porous structure can be obtained.
The invention also provides porous calcium titanate.
The porous calcium titanate is prepared by adopting the eutectic solvent.
The following examples are provided to further illustrate the embodiments of the present invention and are not intended to limit the scope of the present invention.
Example 1
The method for preparing the porous calcium titanate based on the eutectic solvent comprises the following specific steps:
(1) firstly, preparing a eutectic solvent, and uniformly mixing choline chloride and oxalic acid in a molar ratio of 1:1.5 in a beaker to form the eutectic solvent for later use;
(2) grinding and evenly mixing the calcium oxide and the titanium dioxide. Then adding the uniformly ground calcium oxide and titanium dioxide into the eutectic solvent according to the liquid-solid ratio of 1:10 for dissolving, wherein the stirring speed is controlled at 200 revolutions per minute, the temperature is 40 ℃, and the dissolving time is 2 hours;
(3) adding the solution dissolving the raw materials into deionized water with the volume of 10 times of that of the solution, standing and precipitating for 2 hours;
(4) and finally, standing the water-added solution for precipitation, filtering, calcining the generated powder in a tubular furnace, controlling the heating rate to be 2 ℃/min, heating to 900 ℃, calcining for 3h, naturally cooling to room temperature, and taking out to obtain calcium titanate powder with the purity of 99.5 percent by detection.
The XRD and SEM images of the product of this example are shown in fig. 1 and 2. It can be seen from fig. 2 that the resulting product forms a porous structure and is thus a porous calcium carbonate.
Example 2
The method for preparing the porous calcium titanate based on the eutectic solvent comprises the following specific steps:
(1) firstly, preparing a eutectic solvent, and uniformly mixing choline chloride and oxalic acid in a molar ratio of 1:1 in a beaker to form the eutectic solvent for later use;
(2) grinding and evenly mixing the calcium oxide and the titanium dioxide. Then adding the uniformly ground calcium oxide and titanium dioxide into the eutectic solvent according to the liquid-solid ratio of 1:15 for dissolving, wherein the stirring speed is controlled at 100 revolutions per minute, the temperature is 50 ℃, and the dissolving time is 2 hours;
(3) adding the solution dissolving the raw materials into deionized water with the volume of 10 times of that of the solution, standing and precipitating for 2 hours;
(4) and finally, standing the water-added solution for precipitation, filtering, calcining the generated powder in a tubular furnace, controlling the heating rate to be 2 ℃/min, heating to 875 ℃, calcining for 5 hours, naturally cooling to room temperature, and taking out to obtain the porous calcium titanate powder with the purity of 99.6 percent.
Example 3
The method for preparing the porous calcium titanate based on the eutectic solvent comprises the following specific steps:
(1) firstly, preparing a eutectic solvent, and uniformly mixing choline chloride and oxalic acid in a molar ratio of 1:2 in a beaker to form the eutectic solvent for later use;
(2) grinding and evenly mixing the calcium oxide and the titanium dioxide. Then adding the uniformly ground calcium oxide and titanium dioxide into the eutectic solvent according to the liquid-solid ratio of 1:10 for dissolving, wherein the stirring speed is controlled at 400 r/m, the temperature is 50 ℃, and the dissolving time is 1 h;
(3) adding the solution dissolving the raw materials into deionized water with the volume of 10 times of that of the solution, standing and precipitating for 4 hours;
(4) and finally, standing the water-added solution for precipitation, filtering, calcining the generated powder in a tubular furnace, controlling the heating rate to be 5 ℃/min, heating to 925 ℃, calcining for 4h, naturally cooling to room temperature, and taking out to obtain the porous calcium titanate powder with the purity of 99.7%.
Example 4
The method for preparing the porous calcium titanate based on the eutectic solvent comprises the following specific steps:
(1) firstly, preparing a eutectic solvent, and uniformly mixing choline chloride and oxalic acid in a molar ratio of 1:1 in a beaker to form the eutectic solvent for later use;
(2) grinding and evenly mixing the calcium oxide and the titanium dioxide. Then adding the uniformly ground calcium oxide and titanium dioxide into the eutectic solvent according to the liquid-solid ratio of 1:15 for dissolving, wherein the stirring speed is controlled at 50 revolutions per minute, the temperature is 60 ℃, and the dissolving time is 5 hours;
(3) adding the solution dissolving the raw materials into deionized water with the volume of 10 times of that of the solution, standing and precipitating for 3 hours;
(4) and finally, standing the water-added solution for precipitation, filtering, calcining the generated powder in a tubular furnace, controlling the heating rate to be 2 ℃/min, heating to 900 ℃, preserving the heat for 4h, naturally cooling to room temperature, and taking out to obtain the porous calcium titanate powder with the purity of 99.3%.
Example 5
The method for preparing the porous calcium titanate based on the eutectic solvent comprises the following specific steps:
(1) firstly, preparing a eutectic solvent, and uniformly mixing choline chloride and oxalic acid in a molar ratio of 1:1.5 in a beaker to form the eutectic solvent for later use;
(2) grinding and evenly mixing the calcium oxide and the titanium dioxide. Then adding the uniformly ground calcium oxide and titanium dioxide into the eutectic solvent according to the liquid-solid ratio of 1:10 for dissolving, wherein the stirring speed is controlled at 200 revolutions per minute, the temperature is 50 ℃, and the dissolving time is 4 hours;
(3) adding the solution dissolving the raw materials into deionized water with the volume 20 times that of the solution, standing and precipitating for 2 hours;
(4) and finally, standing the water-added solution for precipitation, filtering, calcining the generated powder in a tubular furnace, controlling the heating rate to be 5 ℃/min, heating to 950 ℃, preserving the heat for 5h, naturally cooling to room temperature, and taking out to obtain the porous calcium titanate powder with the purity of 99.4%.
Claims (16)
1. The method for preparing the porous calcium titanate based on the eutectic solvent is characterized by comprising the following steps of:
a. preparing a eutectic solvent: uniformly mixing a hydrogen bond acceptor and a hydrogen bond donor according to the molar ratio of 1-1.5:1-3 to obtain a eutectic solvent; wherein the hydrogen bond acceptor is a quaternary ammonium salt or betaine; the hydrogen bond donor is a carboxylic acid;
b. dissolving raw materials: adding a mixture containing calcium and titanium dioxide into a eutectic solvent according to a liquid-solid ratio of 1:4-30, and mixing for 1-5h at 20-60 ℃ to obtain a mixed solution; wherein the molar ratio of the calcium-containing substance to the titanium dioxide is 1: 1; the calcium-containing substance is calcium oxide or calcium hydroxide;
c. solution dilution and precipitation: uniformly mixing the mixed solution prepared in the step b with water according to the volume ratio of 1:5-20, standing, precipitating and filtering to obtain a solid substance;
d. and (3) calcining: and calcining the solid matter, controlling the heating rate to be 2-5 ℃/min, heating to 875-950 ℃, calcining for 3-5 h, and cooling to room temperature to obtain the porous calcium titanate powder.
2. The method for preparing porous calcium titanate according to claim 1, wherein in the step a: the hydrogen bond acceptor is quaternary ammonium salt.
3. The method for preparing porous calcium titanate according to claim 2, wherein in the step a: the quaternary ammonium salt is at least one of choline chloride and benzyltriethylammonium chloride.
4. The method for preparing porous calcium titanate according to claim 2, wherein in the step a: the hydrogen bond receptor is choline chloride.
5. The method for preparing porous calcium titanate according to claim 1 or 2, wherein in the step a: the hydrogen bond donor is oxalic acid, malic acid, citric acid or succinic acid.
6. The method for preparing porous calcium titanate according to claim 5, wherein in the step a: the hydrogen bond donor is oxalic acid.
7. The method for preparing porous calcium titanate according to claim 1, wherein in the step a: the molar ratio of the hydrogen bond acceptor to the hydrogen bond donor is 1: 1-2.
8. The method for preparing porous calcium titanate according to claim 7, wherein in the step a: the molar ratio of the hydrogen bond acceptor to the hydrogen bond donor is 1: 2.
9. The method for preparing porous calcium titanate according to claim 1, wherein in the step b: the granularity of the calcium-containing substance is less than or equal to 100 meshes, and the granularity of the titanium dioxide is less than or equal to 100 meshes.
10. The method for preparing porous calcium titanate according to claim 1, wherein in the step b: the liquid-solid ratio is 1: 10-15.
11. The method for preparing porous calcium titanate according to claim 10, wherein in the step b: the liquid-solid ratio is 1: 10.
12. The method for preparing porous calcium titanate according to claim 1, wherein in the step b: the temperature is 50 ℃, and the mixing time is 1-5 h.
13. The method for preparing porous calcium titanate according to claim 12, wherein in the step b: the mixing time is 1-2 h.
14. The method for preparing porous calcium titanate according to claim 1, wherein in the step c: the precipitation time is 2-4 h.
15. The method for preparing porous calcium titanate according to claim 1, wherein in step d: heating to 875-925 ℃ and calcining for 4-5 h.
16. The porous calcium titanate according to any one of claims 1 to 15, which is produced by the method for producing porous calcium titanate.
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