CN-121974388-A - Method for synthesizing nano magnesium dititanate by solid phase method

CN121974388ACN 121974388 ACN121974388 ACN 121974388ACN-121974388-A

Abstract

The invention discloses a method for synthesizing nano magnesium dittanate by a solid phase method, which comprises the following steps of S1, weighing a titanium-containing solid compound, nano magnesium oxide solid and a hydrolysis alkaline solid compound, uniformly mixing, adding a surfactant, grinding to obtain a solid mixture, S2, adding a mixed solution with an alcohol-water ratio of 1:1 into the solid mixture, grinding to obtain mixed slurry, S3, transferring the mixed slurry into a centrifuge tube, placing the centrifuge tube into a centrifugal separation machine for centrifugal separation, pouring supernatant after finishing the centrifugal separation, obtaining a mixed product after finishing the water washing process and the alcohol washing process, S4, placing the mixed product into an inorganic acid solution for soaking, transferring the mixture into the centrifuge tube for centrifugal separation, sequentially finishing the water washing process and the alcohol washing process, and then drying to obtain MgO@Ti 2 with a core-shell structure, and S5, calcining the MgO@Ti 2 at high temperature to obtain the nano magnesium dittanate solid.

Inventors

WANG HONGLIANG
WU MIN
YANG XINLU
LI CHENG

Assignees

安徽绿沃循环能源科技有限公司

Dates

Publication Date: 20260505
Application Date: 20251224

Claims (9)

1. A method for synthesizing nano magnesium dititanate by a solid phase method is characterized by comprising the following steps of, S1, weighing a titanium-containing solid compound, a nano magnesium oxide solid and a hydrolysis alkaline solid compound, uniformly mixing in a ceramic mortar, and then adding a surfactant to grind 30-90 min to obtain a solid mixture; S2, adding a mixed solution with an alcohol-water ratio of 1:1 of 3-10 mL into the solid mixture obtained in the step S1, continuously grinding for 60-120min, and obtaining mixed slurry after finishing grinding; S3, transferring the mixed slurry obtained in the step S2 into a centrifuge tube, placing the centrifuge tube for centrifugal separation, pouring out supernatant after the centrifugal separation is finished, and performing a plurality of water washing processes, wherein the water washing process comprises the steps of adding deionized water, stirring for 2-5 min by using a glass rod, centrifuging again, pouring out supernatant after each water washing process is finished, and performing the next water washing process; Pouring out the supernatant after the water washing process is finished, and performing alcohol washing processes for a plurality of times, wherein the alcohol washing process comprises the steps of adding absolute ethanol solution, stirring for 2-5 min by using a glass rod, centrifuging again, pouring out the supernatant after each alcohol washing process is finished, and performing the next alcohol washing process to obtain a mixed product; s4, soaking the mixed product obtained in the step S3 in an inorganic acid solution with a certain mass concentration for 30-120 min, transferring into a centrifuge tube for centrifugal separation, sequentially completing the water washing and alcohol washing processes, and then placing the mixture in a drying oven for constant-temperature drying to obtain MgO@Ti 2 with a core-shell structure; S5, calcining the MgO@TiO 2 obtained in the step S4 at a high temperature to obtain a nano magnesium dititanate solid.
2. The method for synthesizing nano magnesium dititanate according to claim 1, wherein the solid compound containing titanium in step S1 is at least one of titanyl sulfate, titanium hydroxide or titanium alkoxide, and the solid compound containing hydrolyzed alkaline is at least one of sodium carbonate, sodium bicarbonate and urea.
3. The method for synthesizing nano magnesium dititanate according to claim 1, wherein the molar ratio of the titanium-containing solid compound to the nano magnesium oxide solid in step S1 is n (Ti): n (Mg) =2:1, and the molar ratio of the titanium-containing solid compound to the hydrolysis basic solid compound is n (titanium-containing solid compound): n (hydrolysis basic solid compound) =1:1.
4. The method for synthesizing nano magnesium dititanate by solid phase method according to claim 1, wherein the surfactant in the step S1 is at least one of a cationic surfactant, an anionic surfactant and a nonionic surfactant, and the amount of the surfactant is 1% -10% of the total mass of the reactants.
5. The method for synthesizing nano magnesium dititanate by solid phase method according to claim 1, wherein the number of water washing times in the steps S3 and S4 is 3-5 times, and the number of alcohol washing times is 3-5 times.
6. The method for synthesizing nano magnesium dititanate according to claim 1, wherein the mineral acid solution in step S4 is at least one of hydrochloric acid, sulfuric acid and nitric acid, and the concentration is 0.1-0.5 mol/L.
7. The method for synthesizing nano magnesium dititanate by solid phase method according to claim 1, wherein the constant temperature drying in step S4 is 80-120 ℃ for 3-6 h.
8. The method for synthesizing nano magnesium dititanate according to claim 1, wherein the calcining temperature in step S5 is 500-950 ℃ and the time is 60-150 min.
9. The method for synthesizing nano magnesium dititanate by the solid phase method according to claim 1, wherein in the step S5, mgO@TiO 2 obtained in the step S4 is put into a muffle furnace for high-temperature calcination to obtain nano magnesium dititanate solid.

Description

Method for synthesizing nano magnesium dititanate by solid phase method Technical Field The invention relates to the technical field of nano magnesium dititanate synthesis, in particular to a method for synthesizing nano magnesium dititanate by a solid phase method. Background Magnesium dititanate ((MgTi 2O5) has the characteristics of good thermal stability, high refractive index, high dielectric constant, low cost, no dielectric loss and the like, not only can improve the impact resistance and the thermal strain capacity of a ceramic material, but also can enable the ceramic structure to be highly compact so as to avoid the influence caused by the dielectric loss. The preparation method of the nano magnesium dititanate mainly comprises a solid phase method, a liquid phase method and a gas phase method. The gas phase method can obtain high-purity and less-agglomeration products, but the required equipment is complex, the cost is extremely high, the method is generally not specially required to be rarely adopted, the liquid phase method can prepare MgTi 2O5 powder with good relative purity and uniformity, but compared with the solid phase method, the method has the characteristics of complex operation, long period, high cost and inapplicability to industrial production, the solid phase method has the characteristics of low cost, simple operation and short period, but the obtained powder has large particle size (micron level), non-uniform chemical composition and low product purity, and the improvement of material performance is limited. Disclosure of Invention The invention aims to provide a method for synthesizing nano magnesium dititanate by a solid phase method, which is simple and convenient to operate, low in cost, environment-friendly and easy for industrial production, and solves the problems of large particle size and non-uniform chemical composition of magnesium dititanate powder prepared by the solid phase method in the prior art. In order to achieve the above purpose, the present invention provides the following technical solutions: a method for synthesizing nano magnesium dititanate by a solid phase method, which comprises the following steps, S1, weighing a titanium-containing solid compound, a nano magnesium oxide solid and a hydrolysis alkaline solid compound, uniformly mixing in a ceramic mortar, and then adding a surfactant to grind 30-90 min to obtain a solid mixture; S2, adding a mixed solution with an alcohol-water ratio of 1:1 of 3-10 mL into the solid mixture obtained in the step S1, continuously grinding for 60-120min, and obtaining mixed slurry after finishing grinding; S3, transferring the mixed slurry obtained in the step S2 into a centrifuge tube, placing the centrifuge tube for centrifugal separation, pouring out supernatant after the centrifugal separation is finished, and performing a plurality of water washing processes, wherein the water washing process comprises the steps of adding deionized water, stirring for 2-5 min by using a glass rod, centrifuging again, pouring out supernatant after each water washing process is finished, and performing the next water washing process; Pouring out the supernatant after the water washing process is finished, and performing alcohol washing processes for a plurality of times, wherein the alcohol washing process comprises the steps of adding absolute ethanol solution, stirring for 2-5 min by using a glass rod, centrifuging again, pouring out the supernatant after each alcohol washing process is finished, and performing the next alcohol washing process to obtain a mixed product; S4, soaking the mixed product obtained in the step S3 in an inorganic acid solution with a certain mass concentration for 30-120 min, transferring into a centrifuge tube for centrifugal separation, sequentially completing the water washing and alcohol washing processes, and then placing the mixture in a drying oven for constant-temperature drying to obtain MgO@TiO2 with a core-shell structure; S5, calcining the MgO@TiO2 obtained in the step S4 at a high temperature to obtain a nano magnesium dititanate solid. Preferably, the solid compound containing titanium in step S1 is at least one of titanyl sulfate, titanium hydroxide or titanium alkoxide, and the solid compound containing hydrolysis is at least one of sodium carbonate, sodium bicarbonate and urea. Preferably, the molar ratio of the titanium-containing solid compound to the nano magnesium oxide solid in the step S1 is n (Ti): n (Mg) =2:1, and the molar ratio of the titanium-containing solid compound to the hydrolysis basic solid compound is n (titanium-containing solid compound) =1:1. Preferably, the surfactant in the step S1 is at least one of a cationic surfactant, an anionic surfactant or a nonionic surfactant, and the amount of the surfactant is 1% -10% of the total mass of the reactants. Preferably, the number of water washes described in steps S3 and S4 is 3-5 and the number of alcohol washes is 3-5. Pre