CN108910951B - Preparation method of titanium dioxide and molybdenum trioxide composite powder - Google Patents
Preparation method of titanium dioxide and molybdenum trioxide composite powder Download PDFInfo
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Abstract
The invention discloses a preparation method of titanium dioxide and molybdenum trioxide composite powder, which is characterized by dissolving titanyl ammonium oxalate monohydrate and ammonium molybdate in ammonia water to realize the molecular level diffusion motion mixing of titanium and molybdenum in an occurrence state to form a titanyl ammonium oxalate monohydrate-ammonium molybdate uniform solution, dehydrating the titanyl ammonium oxalate monohydrate-ammonium molybdate solution in a spray drying mode to realize the purpose of preparing the titanyl ammonium oxalate monohydrate-ammonium molybdate uniform composite powder from the titanyl ammonium oxalate monohydrate-ammonium molybdate solution, then carrying out crushing and screening treatment by a high-speed universal crusher, and finally carrying out high-temperature treatment to thermally decompose the titanyl ammonium oxalate monohydrate-ammonium molybdate to prepare the titanium dioxide and molybdenum trioxide composite powder with uniform titanium dioxide distribution and good product consistency.
Description
Technical Field
The invention belongs to the technical field of composite material preparation methods, and particularly relates to a preparation method of titanium dioxide and molybdenum trioxide composite powder.
Background
Molybdenum trioxide is an important intermediate product in a molybdenum metallurgy industrial chain, the quality of the molybdenum trioxide directly influences the quality and the processing technology of downstream products such as molybdenum powder and molybdenum catalysts prepared from molybdenum trioxide, the content, the particle size and the particle size distribution of molybdenum trioxide are accurately measured, the morphology of molybdenum trioxide crystals is determined, and the molybdenum trioxide is particularly important for evaluating the quality of molybdenum trioxide products.
The atomic absorption method for determining the content of metal titanium in molybdenum trioxide needs to use titanium dioxide and molybdenum trioxide composite powder as a basic sample, and the uniformity of the element content of the titanium dioxide and molybdenum trioxide composite powder influences the accuracy of molybdenum trioxide determination, so that the accuracy of quality evaluation of molybdenum trioxide is influenced, and the subsequent processing technology and product quality of molybdenum trioxide are caused.
At present, liquid-solid or solid-solid mechanical mixing methods are generally adopted for preparing lanthanum-molybdenum, strontium-molybdenum, titanium-molybdenum metal alloy powder, rare earth molybdenum oxide and molybdenum oxide composite powder. The preparation of lanthanum-molybdenum dioxide composite powder is taken as an example to illustrate the defects of the liquid-solid or solid-solid mechanical mixing method. Preparing lanthanum-molybdenum oxide powder by a liquid-solid mechanical mixing method: firstly, converting lanthanum oxide into a lanthanum nitrate solution; secondly, adding the lanthanum nitrate solution into the molybdenum dioxide in a stirring state by a spraying method; thirdly, stirring and drying the wet mixture of molybdenum dioxide and lanthanum nitrate; fourthly, crushing and sieving the mixture of molybdenum dioxide and lanthanum nitrate; fifthly, mixing undersize materials of the mixture of the molybdenum dioxide and the lanthanum nitrate to obtain lanthanum-molybdenum dioxide powder. Preparing lanthanum-molybdenum oxide powder by a solid-solid mechanical mixing method: firstly, dispersing nano lanthanum oxide in a solution; secondly, spraying the nano lanthanum oxide dispersion suspension to the molybdenum dioxide in a stirring state in a spraying mode; thirdly, stirring and drying the molybdenum dioxide-lanthanum oxide-water material prepared in the step two; (IV) crushing and sieving the molybdenum dioxide-lanthanum oxide mixture prepared in the step (III); and (V) mixing the undersize products obtained in the step (IV) to obtain the lanthanum oxide-molybdenum dioxide powder.
Obviously, when the titanium dioxide and molybdenum trioxide composite powder is prepared by a liquid-solid mechanical mixing method or a solid-solid mechanical mixing method, the diffusion power between the titanium dioxide and the molybdenum trioxide is insufficient, so that the prepared powder material has poor uniformity. The specific reason is analyzed as follows: firstly, titanium dioxide and molybdenum trioxide are mechanically mixed and lack diffusion movement at a molecular level, so that the titanium dioxide and the molybdenum trioxide cannot be uniformly distributed; secondly, when the titanium dioxide and the molybdenum trioxide are mechanically mixed, larger particle steric hindrance exists, and the mutual distribution non-uniformity of the titanium dioxide and the molybdenum trioxide is further increased; third, mechanical mixing operational errors exacerbate the non-uniformity of the mutual distribution of titanium dioxide and molybdenum trioxide.
Therefore, a preparation method of titanium dioxide and molybdenum trioxide composite powder, which has sufficient mutual diffusion power of titanium dioxide and molybdenum trioxide, uniform distribution of titanium dioxide in a molybdenum trioxide matrix and good product consistency, needs to be developed.
Disclosure of Invention
The invention aims to provide a preparation method of titanium dioxide and molybdenum trioxide composite powder, and provides a preparation method of titanium dioxide and molybdenum trioxide composite powder with uniform distribution and good product consistency.
The invention adopts the technical scheme that a preparation method of titanium dioxide and molybdenum trioxide composite powder specifically comprises the following steps:
step 1, preparing a titanyl ammonium hydrogen oxalate monohydrate solution: adding deionized water into a beaker, continuously adding titanyl ammonium oxalate monohydrate, and stirring to completely dissolve the titanyl ammonium oxalate monohydrate in the deionized water to obtain a titanyl ammonium oxalate monohydrate solution;
step 2, preparing an ammonium molybdate solution: respectively weighing ammonia water and deionized water, adding into the same beaker, placing the beaker on an electric heating sleeve and stirring, continuously adding molybdenum trioxide, then starting heating with the electric heating sleeve, heating and stirring MoO3-H2O-NH4Completely dissolving molybdenum trioxide to be clear by using an OH mixture to obtain an ammonium molybdate solution;
step 3, preparing a titanyl ammonium oxalate monohydrate-ammonium molybdate solution: adding the titanyl ammonium oxalate monohydrate solution into the ammonium molybdate solution, and stirring for 1-3 h at the temperature of 65-90 ℃ to obtain the titanyl ammonium oxalate monohydrate-ammonium molybdate solution;
step 4, preparing titanyl ammonium hydrogen oxalate-ammonium molybdate composite powder: carrying out spray dehydration on the titanyl ammonium oxalate monohydrate-ammonium molybdate solution to obtain titanyl ammonium oxalate monohydrate-ammonium molybdate composite powder;
step 5, preparing the titanyl ammonium oxalate monohydrate-ammonium molybdate composite powder with a certain granularity: crushing the titanyl ammonium oxalate monohydrate-ammonium molybdate composite powder by using a high-speed crusher, and screening the crushed titanyl ammonium oxalate monohydrate-ammonium molybdate composite powder by using a screen, wherein the screened titanyl ammonium oxalate monohydrate-ammonium molybdate composite powder has a certain particle size;
and 6, putting the titanyl ammonium oxalate monohydrate-ammonium molybdate composite powder with a certain granularity into a stainless steel material boat, and finally putting the stainless steel material boat into a heating furnace for heating to obtain the titanium dioxide and molybdenum trioxide composite powder.
The invention is also characterized in that:
in the step 1, the mass of the titanyl ammonium monohydrochloride is 0.0412 to 16.4609g, and the mass of the deionized water is 50 to 550 g.
In the step 2, the mass ratio of the ammonia water to the deionized water is 1:1-1:3, the mass ratio of the molybdenum trioxide to the deionized water is 1:1-1:3, and the mass percentage of the ammonium titanyl oxalate monohydrate to the molybdenum trioxide is 0.0041-1.6461%.
In the step 2, a mechanical stirring device is used for stirring, the stirring speed is 280-500r/min, and the heating temperature is 65-85 ℃.
And stirring in the step 3 by using a mechanical stirring device, wherein the stirring speed is controlled to be 280-500 r/min.
And 4, performing spray dehydration treatment by using a spray drying tower, wherein the temperature of an air inlet of the spray drying tower is 210-260 ℃, the temperature of an air outlet of the spray drying tower is 115-150 ℃, and the rotating speed of an atomizer of the spray drying tower is 0.5 × 104-2.2×104r/min。
The rotation speed of the high-speed pulverizer in the step 5 is 0.5 × 104-2.0×104r/min, the mesh number of the sieve is 80-160 meshes.
And 6, putting the titanyl ammonium oxalate monohydrate-ammonium molybdate composite powder with a certain granularity into a stainless steel material boat, wherein the thickness of the titanyl ammonium oxalate monohydrate-ammonium molybdate composite powder is 0.5-1.2 cm.
In step 6, the temperature in the heating furnace is distributed in a gradient manner in the horizontal direction, and is sequentially 350-360 ℃, 410-420 ℃, 470-480 ℃ and 450-460 ℃, and the heating time of the stainless steel material boat in the heating furnace is 3-5 h.
The invention has the beneficial effects that: according to the preparation method of the titanium dioxide and molybdenum trioxide composite powder, the ammonium titanyl oxalate and the ammonium molybdate realize molecular-level diffusion motion in a water-ammonia system, and molecular-level mixing is realized, compared with liquid-solid or solid-solid mechanical mixing, the mixing power tends to be infinite, and the mixing resistance tends to be infinite, so that the uniformity degree of the prepared titanium dioxide-molybdenum trioxide powder is qualitatively improved, and the uniformity of a spectral standard molybdenum trioxide sample for measuring the content of molybdenum trioxide and titanium is ensured.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
The invention relates to a preparation method of titanium dioxide and molybdenum trioxide composite powder, which comprises the following steps:
step 1, adding deionized water into a beaker, continuously adding titanyl ammonium oxalate monohydrate, and stirring to completely dissolve the titanyl ammonium oxalate monohydrate into the deionized water to obtain a titanyl ammonium oxalate monohydrate solution, wherein the mass ratio of the titanyl ammonium oxalate monohydrate to the deionized water is 1: 3-1: 13000.
step 2, respectively weighing ammonia water and deionized water, adding the ammonia water and the deionized water into a beaker, placing the beaker on an electric heating sleeve, stirring, continuously adding molybdenum trioxide, then starting heating by using the electric heating sleeve, heating and continuously stirring MoO3-H2O-NH4Completely dissolving molybdenum trioxide to be clear by using an OH mixture to obtain an ammonium molybdate solution, wherein the mass ratio of ammonia water to deionized water is 1:1-1:3, the mass ratio of molybdenum trioxide to deionized water is 1:1-1:3, the mass percentage of ammonium titanyl oxalate to molybdenum trioxide is 0.0041-1.6461%, stirring by using a mechanical stirring device at a stirring speed of 280-500r/min and a heating temperature of 65-85 ℃;
step 3, adding the titanyl ammonium oxalate monohydrate solution into the ammonium molybdate solution, stirring for 1-3 h at 65-90 ℃ to obtain the titanyl ammonium oxalate monohydrate-ammonium molybdate solution, stirring by using a mechanical stirring device during stirring, and controlling the stirring speed to be 280-500 r/min;
step 4, carrying out spray dehydration on the titanyl ammonium oxalate monohydrate-ammonium molybdate solution by using a spray drying tower to obtain a titanyl ammonium oxalate monohydrate-ammonium molybdate compound, wherein the air inlet temperature of the spray drying tower is 210-260 ℃, the air outlet temperature is 115-150 ℃, and the rotating speed of an atomizer of the spray drying tower is 0.5 × 104-2.2×104r/min；
And 5, crushing the titanyl ammonium oxalate monohydrate-ammonium molybdate compound by using a high-speed crusher, and screening the crushed titanyl ammonium oxalate monohydrate-ammonium molybdate compound by using a screen, wherein the screened titanyl ammonium oxalate monohydrate-ammonium molybdate compound powder is titanyl ammonium molybdate monohydrate-ammonium molybdate compound powder, and the rotating speed of the high-speed crusher is 0.5 × 104-2.0×104r/min, the mesh number of the sieve is 80-160 meshes;
and 6, putting the titanyl ammonium oxalate monohydrate-ammonium molybdate composite powder into a stainless steel material boat, and finally putting the stainless steel material boat into a heating furnace with the temperature in gradient distribution to heat for 3-5 hours to obtain the titanium dioxide and molybdenum trioxide composite powder, wherein the thickness of the titanyl ammonium oxalate monohydrate-ammonium molybdate composite powder in the stainless steel material boat is 0.5-1.2cm, and the temperature in the heating furnace is in gradient distribution in the horizontal direction and is 350-360 ℃, 410-420 ℃, 470-480 ℃ and 450-460 ℃ in sequence.
Example 1
Step 1, adding 50g of deionized water into a beaker, continuously adding 0.0412g of titanyl ammonium monohydroxyoxalate, and stirring with a glass rod to completely dissolve the titanyl ammonium monohydroxyoxalate in the deionized water to obtain a titanyl ammonium monohydroxyoxalate solution;
step 2, respectively weighing 1000g of ammonia water and 1000g of deionized water, adding the ammonia water and the deionized water into the same beaker, then placing the beaker on an electric heating sleeve and mechanically stirring the mixture at the stirring speed of 280r/min, continuously adding 1000g of molybdenum trioxide, then starting heating the mixture by the electric heating sleeve, heating and stirring MoO3-H2O-NH4The OH mixture is heated to 65 ℃ to completely dissolve the molybdenum trioxide until the molybdenum trioxide is clear, so as to obtain an ammonium molybdate solution;
step 3, adding the titanyl ammonium oxalate monohydrate solution into an ammonium molybdate solution, and stirring for 1h at 65 ℃ to obtain the titanyl ammonium oxalate monohydrate-ammonium molybdate solution;
step 4, carrying out spray dehydration on the titanyl ammonium oxalate monohydrate-ammonium molybdate solution by using a spray drying tower, controlling the temperature of an air inlet of the spray drying tower to be 210 ℃, the temperature of an air outlet to be 115 ℃, and controlling the rotating speed of an atomizer of the spray drying tower to be 0.5 × 104r/min to obtain a titanyl ammonium oxalate monohydrate-ammonium molybdate compound;
step 5, crushing the titanyl ammonium hydrogen oxalate-ammonium molybdate compound by using a high-speed crusher, wherein the rotating speed of the high-speed crusher is controlled to be 1.9 × 104r/min; secondly, screening the crushed titanyl ammonium oxalate monohydrate-ammonium molybdate compound by using a sieve with a certain mesh of 160 to obtain a 160-mesh screen underflow, namely titanyl ammonium oxalate monohydrate-ammonium molybdate compound powder;
and 6, putting the 160-mesh titanyl ammonium oxalate-ammonium molybdate composite powder into a stainless steel material boat, wherein the thickness of the titanyl ammonium oxalate-ammonium molybdate composite powder is 0.5cm, and putting the stainless steel material boat into a heating furnace which is in gradient distribution in the temperature horizontal direction and sequentially has the temperature of 350-360 ℃, 410-420 ℃, 470-480 ℃ and 450-460 ℃ for heating for 3 hours to obtain the titanium dioxide and molybdenum trioxide composite powder.
Example 2
Step 1, adding 100g of deionized water into a beaker, continuously adding 0.9936g of titanyl ammonium oxalate monohydrate, and stirring with a glass rod to completely dissolve the titanyl ammonium oxalate monohydrate into the deionized water to obtain a titanyl ammonium oxalate monohydrate solution;
step 2, respectively weighing 1000g of ammonia water and 2500g of deionized water, adding the ammonia water and the deionized water into a beaker, then placing the beaker on an electric heating sleeve and mechanically stirring the mixture at the stirring speed of 460r/min, continuously adding 1000g of molybdenum trioxide, then starting heating the mixture by the electric heating sleeve, heating the mixture and stirring MoO3-H2O-NH4The OH mixture is heated to 79 ℃ to completely dissolve the molybdenum trioxide until the molybdenum trioxide is clear, so as to obtain an ammonium molybdate solution;
step 3, adding the titanyl ammonium oxalate monohydrate solution into the ammonium molybdate solution, and stirring for 3 hours at 86 ℃ to obtain the titanyl ammonium oxalate monohydrate-ammonium molybdate solution;
step 4, carrying out spray dehydration on the titanyl ammonium oxalate monohydrate-ammonium molybdate solution by using a spray drying tower, controlling the temperature of an air inlet of the spray drying tower to be 239 ℃, the temperature of an air outlet of the spray drying tower to be 136 ℃, and controlling the rotating speed of an atomizer of the spray drying tower to be 2.0 × 104r/min to obtain a titanyl ammonium oxalate monohydrate-ammonium molybdate compound;
step 5, crushing the titanyl ammonium hydrogen oxalate-ammonium molybdate compound by using a high-speed crusher to obtain high-speed powderThe rotating speed of the crusher is controlled to be 1.9 × 104r/min; secondly, screening the crushed titanyl ammonium oxalate monohydrate-ammonium molybdate compound by using a sieve with a certain mesh of 160 to obtain a 160-mesh screen underflow, namely titanyl ammonium oxalate monohydrate-ammonium molybdate compound powder;
and 6, putting the 160-mesh titanyl ammonium oxalate-ammonium molybdate composite powder into a stainless steel material boat, wherein the thickness of the titanyl ammonium oxalate-ammonium molybdate composite powder is 0.5cm, and putting the stainless steel material boat into a heating furnace which is in gradient distribution in the temperature horizontal direction and sequentially has the temperature of 350-360 ℃, 410-420 ℃, 470-480 ℃ and 450-460 ℃ for heating for 3 hours to obtain the titanium dioxide and molybdenum trioxide composite powder.
Example 3
Step 1, adding 350g of deionized water into a beaker, continuously adding 4.5706g of titanyl ammonium monohydroxyoxalate, and stirring with a glass rod to completely dissolve the titanyl ammonium monohydroxyoxalate in the deionized water to obtain a titanyl ammonium monohydroxyoxalate solution;
step 2, respectively weighing 1000g of ammonia water and 1500g of deionized water, adding the ammonia water and the deionized water into a beaker, then placing the beaker on an electric heating sleeve and mechanically stirring the mixture at the stirring speed of 360r/min, continuously adding 1000g of molybdenum trioxide, then starting heating the mixture by the electric heating sleeve, heating and stirring MoO3-H2O-NH4The OH mixture is heated to 70 ℃ to completely dissolve the molybdenum trioxide until the molybdenum trioxide is clear, so as to obtain an ammonium molybdate solution;
step 3, adding the titanyl ammonium oxalate monohydrate solution into an ammonium molybdate solution, and stirring for 1.5 hours at the temperature of 70 ℃ to obtain the titanyl ammonium oxalate monohydrate-ammonium molybdate solution;
step 4, carrying out spray dehydration on the titanyl ammonium oxalate monohydrate-ammonium molybdate solution by using a spray drying tower, controlling the temperature of an air inlet of the spray drying tower to be 230 ℃, the temperature of an air outlet of the spray drying tower to be 120 ℃, and controlling the rotating speed of an atomizer of the spray drying tower to be 1.3 × 104r/min to obtain a titanyl ammonium oxalate monohydrate-ammonium molybdate compound;
step 5, crushing the titanyl ammonium hydrogen oxalate-ammonium molybdate compound by using a high-speed crusher, wherein the rotating speed of the high-speed crusher is controlled to be 1.5 × 104r/min; then sieving the crushed oxalic acid monohydrate by a sieve with a certain 120 meshesObtaining a 120-mesh screen underflow substance, namely the titanyl ammonium oxalate-ammonium molybdate composite powder;
and 6, putting the 120-mesh titanyl ammonium oxalate-ammonium molybdate composite powder into a stainless steel material boat, wherein the thickness of the titanyl ammonium oxalate-ammonium molybdate composite powder is 0.8cm, and putting the stainless steel material boat into a heating furnace which is in gradient distribution in the temperature horizontal direction and sequentially has the temperature of 350-360 ℃, 410-420 ℃, 470-480 ℃ and 450-460 ℃ for heating for 3.5h to obtain the titanium dioxide and molybdenum trioxide composite powder.
Example 4
Step 1, adding 400g of deionized water into a beaker, continuously adding 10.3572g of titanyl ammonium monohydroxyoxalate, and stirring with a glass rod to completely dissolve the titanyl ammonium monohydroxyoxalate in the deionized water to obtain a titanyl ammonium monohydroxyoxalate solution;
step 2, respectively weighing 1000g of ammonia water and 2000g of deionized water, adding the ammonia water and the deionized water into a beaker, then placing the beaker on an electric heating sleeve and mechanically stirring the mixture at the stirring speed of 400r/min, continuously adding 1000g of molybdenum trioxide, then starting heating the mixture by the electric heating sleeve, heating and stirring MoO3-H2O-NH4The OH mixture is heated to 76 ℃ to completely dissolve the molybdenum trioxide until the molybdenum trioxide is clear, so as to obtain an ammonium molybdate solution;
step 3, adding the titanyl ammonium oxalate monohydrate solution into an ammonium molybdate solution, and stirring for 1.5 hours at 83 ℃ to obtain the titanyl ammonium oxalate monohydrate-ammonium molybdate solution;
step 4, carrying out spray dehydration on the titanyl ammonium oxalate monohydrate-ammonium molybdate solution by using a spray drying tower, controlling the temperature of an air inlet of the spray drying tower to be 235 ℃, the temperature of an air outlet to be 121 ℃, and controlling the rotating speed of an atomizer of the spray drying tower to be 1.6 × 104r/min to obtain a titanyl ammonium oxalate monohydrate-ammonium molybdate compound;
step 5, crushing the titanyl ammonium hydrogen oxalate-ammonium molybdate compound by using a high-speed crusher, wherein the rotating speed of the high-speed crusher is controlled to be 1.5 × 104r/min; secondly, sieving the crushed titanyl ammonium oxalate monohydrate-ammonium molybdate compound by using a sieve with a certain mesh of 120 to obtain a 120-mesh screen underflow, namely the titanyl ammonium oxalate monohydrate-ammonium molybdate compound powder；
And 6, putting the 120-mesh titanyl ammonium oxalate-ammonium molybdate composite powder into a stainless steel material boat, wherein the thickness of the titanyl ammonium oxalate-ammonium molybdate composite powder is 1.0cm, and putting the stainless steel material boat into a heating furnace which is in gradient distribution in the temperature horizontal direction and sequentially has the temperature of 350-360 ℃, 410-420 ℃, 470-480 ℃ and 450-460 ℃ for heating for 4 hours to obtain the titanium dioxide and molybdenum trioxide composite powder.
Example 5
Step 1, adding 500g of deionized water into a beaker, continuously adding 16.4609g g g of titanyl ammonium oxalate monohydrate, and stirring with a glass rod to completely dissolve the titanyl ammonium oxalate monohydrate in the deionized water to obtain a titanyl ammonium oxalate monohydrate solution;
step 2, respectively weighing 1000g of ammonia water and 3000g of deionized water, adding the ammonia water and the deionized water into a beaker, then placing the beaker on an electric heating sleeve and mechanically stirring the mixture at the stirring speed of 500r/min, continuously adding 1000g of molybdenum trioxide, then starting heating the mixture by the electric heating sleeve, heating and stirring MoO3-H2O-NH4The OH mixture is heated to 85 ℃, so that the molybdenum trioxide is completely dissolved until the molybdenum trioxide is clear, and an ammonium molybdate solution is obtained;
step 3, adding the titanyl ammonium oxalate monohydrate solution into an ammonium molybdate solution, and stirring for 3 hours at 90 ℃ to obtain the titanyl ammonium oxalate monohydrate-ammonium molybdate solution;
step 4, carrying out spray dehydration on the titanyl ammonium oxalate monohydrate-ammonium molybdate solution by using a spray drying tower, controlling the temperature of an air inlet of the spray drying tower to be 255 ℃, the temperature of an air outlet of the spray drying tower to be 148 ℃, and controlling the rotating speed of an atomizer of the spray drying tower to be 2.1 × 104r/min to obtain a titanyl ammonium oxalate monohydrate-ammonium molybdate compound;
step 5, crushing the titanyl ammonium hydrogen oxalate-ammonium molybdate compound by using a high-speed crusher, wherein the rotating speed of the high-speed crusher is controlled to be 2.0 × 104r/min; secondly, screening the crushed titanyl ammonium monohydroxyoxalate-ammonium molybdate compound by using a sieve with a certain 80 meshes to obtain a screen underflow with a 80 meshes, namely titanyl ammonium monohydroxyoxalate-ammonium molybdate compound powder;
and 6, putting 80-mesh titanyl ammonium oxalate-ammonium molybdate composite powder into a stainless steel material boat, wherein the thickness of the titanyl ammonium oxalate-ammonium molybdate composite powder is 1.2cm, and putting the stainless steel material boat into a heating furnace which is in gradient distribution in the temperature horizontal direction and sequentially has the temperature of 350-360 ℃, 410-420 ℃, 470-480 ℃ and 450-460 ℃ for heating for 5 hours to obtain the titanium dioxide and molybdenum trioxide composite powder.
The molybdenum trioxide used in examples 1 to 5 contained 66.53% of molybdenum trioxide, 98% of titanyl ammonium monohydroxyoxalate, 25 to 28% of reagent ammonia, 0.1231% of titanium metal and 66.38% of molybdenum in the composite powder of titanium dioxide and molybdenum trioxide.
Claims (5)
1. A preparation method of titanium dioxide and molybdenum trioxide composite powder is characterized by comprising the following steps: the method specifically comprises the following steps:
step 1, adding deionized water into a beaker, and continuously adding titanyl ammonium oxalate monohydrate, wherein the mass ratio of the titanyl ammonium oxalate monohydrate to deionized water is 1: 3-1: 13000, stirring to completely dissolve the titanyl ammonium oxalate monohydrate in the deionized water to obtain a titanyl ammonium oxalate monohydrate solution;
step 2, respectively weighing ammonia water and deionized water, adding the ammonia water and the deionized water into a beaker, placing the beaker on an electric heating sleeve, stirring, continuously adding molybdenum trioxide, then starting heating by using the electric heating sleeve, and continuously stirring MoO3-H2O-NH4Completely dissolving molybdenum trioxide to be clear by using an OH mixture to obtain an ammonium molybdate solution;
the mass ratio of ammonia water to deionized water is 1:1-1:3, the mass ratio of molybdenum trioxide to deionized water is 1:1-1:3, and the mass percentage of the ammonium titanyl oxalate monohydrate to the molybdenum trioxide is 0.0041-1.6461%;
step 3, adding the titanyl ammonium oxalate monohydrate solution into the ammonium molybdate solution, and stirring for 1-3 h at the temperature of 65-90 ℃ to obtain the titanyl ammonium oxalate monohydrate-ammonium molybdate solution;
step 4, carrying out spray dehydration on the titanyl ammonium oxalate monohydrate-ammonium molybdate solution to obtain a titanyl ammonium oxalate monohydrate-ammonium molybdate compound;
spray dehydration treatment using a spray drying tower, said spray dryingThe temperature of the air inlet of the tower is 210-260 ℃, the temperature of the air outlet is 115-150 ℃, and the rotating speed of the atomizer of the spray drying tower is 0.5 × 104-2.2×104r/min；
Step 5, crushing the titanyl ammonium oxalate monohydrate-ammonium molybdate compound by using a high-speed crusher, and screening the crushed titanyl ammonium oxalate monohydrate-ammonium molybdate compound by using a screen, wherein the screened titanyl ammonium oxalate monohydrate-ammonium molybdate compound is titanyl ammonium molybdate monohydrate composite powder;
step 6, putting the titanyl ammonium oxalate monohydrate-ammonium molybdate composite powder into a stainless steel material boat, and finally putting the stainless steel material boat into a heating furnace for heating to obtain titanium dioxide and molybdenum trioxide composite powder;
the temperature in the heating furnace is distributed in a gradient manner in the horizontal direction, and is sequentially 350-360 ℃, 410-420 ℃, 470-480 ℃ and 450-460 ℃, and the heating time of the stainless steel material boat in the heating furnace is 3-5 h.
2. The method for preparing the titanium dioxide and molybdenum trioxide composite powder according to claim 1, which is characterized in that: and stirring in the step 2 by using a mechanical stirring device, wherein the stirring speed is 280-500r/min, and the heating temperature is 65-85 ℃.
3. The method for preparing the titanium dioxide and molybdenum trioxide composite powder according to claim 1, which is characterized in that: and stirring in the step 3 by using a mechanical stirring device, wherein the stirring speed is controlled to be 280-500 r/min.
4. The method for preparing a titanium dioxide-molybdenum trioxide composite powder according to claim 1, wherein the rotation speed of the high-speed pulverizer in the step 5 is 0.5 × 104-2.0×104r/min, the mesh number of the sieve is 80-160 meshes.
5. The method for preparing the titanium dioxide and molybdenum trioxide composite powder according to claim 1, which is characterized in that: and in the step 6, the thickness of the titanyl ammonium oxalate monohydrate-ammonium molybdate composite powder put into the stainless steel material boat is 0.5-1.2 cm.
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