CN108910951A - A kind of preparation method of titanium dioxide and molybdenum trioxide composite granule - Google Patents
A kind of preparation method of titanium dioxide and molybdenum trioxide composite granule Download PDFInfo
- Publication number
- CN108910951A CN108910951A CN201810618330.5A CN201810618330A CN108910951A CN 108910951 A CN108910951 A CN 108910951A CN 201810618330 A CN201810618330 A CN 201810618330A CN 108910951 A CN108910951 A CN 108910951A
- Authority
- CN
- China
- Prior art keywords
- ammonium
- water plant
- plant acid
- acid titanyl
- molybdenum trioxide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/02—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/08—Drying; Calcining ; After treatment of titanium oxide
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Catalysts (AREA)
Abstract
The invention discloses the preparation methods of a kind of titanium dioxide and molybdenum trioxide composite granule, by a water plant acid titanyl ammonium, ammonium molybdate is dissolved in ammonium hydroxide, realize titanium, the mixing of molybdenum occurrence status molecule rank diffusion motion, form a water plant acid titanyl ammonium-ammonium molybdate homogeneous solution, then a water plant acid titanyl ammonium-ammonium molybdate solution is dehydrated in a manner of being spray-dried, it realizes a water plant acid titanyl ammonium-ammonium molybdate and prepares a water plant acid titanyl ammonium-uniform composite granule purpose of ammonium molybdate from solution, then high speed Universal pulverizer crushing is carried out again, screening process, final high temperature processing thermally decomposes a water plant acid titanyl ammonium-ammonium molybdate, a kind of titanium dioxide has been prepared to be evenly distributed, the titanium dioxide and molybdenum trioxide composite granule of good product consistency.
Description
Technical field
The invention belongs to composite material and preparation method thereof technical fields, and in particular to a kind of titanium dioxide and molybdenum trioxide are compound
Raw powder's production technology.
Background technique
Molybdenum trioxide is an important intermediate products on molybdenum Metallurgical industry chain, and quality directly affects molybdenum trioxide preparation
The downstream product qualities such as molybdenum powder, molybdenum series catalyst and processing technology, Accurate Determining molybdenum trioxide constituent content, granule size, grain
Degree distribution determines molybdenum trioxide crystal morphology, and to carrying out, evaluation molybdenum trioxide product quality is particularly important.
Metal Ti content is needed using titanium dioxide and molybdenum trioxide composite powder in atom absorption method measurement molybdenum trioxide
For body as basic sample, it is quasi- that the uniformity of the constituent content of titanium dioxide and molybdenum trioxide composite granule influences measurement molybdenum trioxide
True property, and then the accuracy of molybdenum trioxide quality evaluation is influenced, cause molybdenum trioxide subsequent machining technology and product quality.
It is generally adopted currently, preparing lanthanum-molybdenum, strontium-molybdenum, titanium-molybdenum metal alloy powder, rare-earth oxidation molybdenum and molybdenum oxide composite granule
With liquid-solid or solid-solid mechanical mix techniques.Illustrate that liquid-solid or solid-solid is mechanical for preparing lanthanum-molybdenum dioxide composite granule
The deficiency of mixed method.Liquid-solid mechanical mix techniques prepare lanthanum-molybdenum oxide powder：Firstly, it is molten to convert lanthanum nitrate for lanthana
Liquid；Secondly, lanthanum nitrate hexahydrate is added with spray method to the molybdenum dioxide of stirring；Third, by wet molybdenum dioxide
With lanthanum nitrate mixture stirring and drying；4th, molybdenum dioxide and lanthanum nitrate mixture crush, are sieved；5th, by molybdenum dioxide and
Lanthanum nitrate mixture screenings mixing, obtains lanthanum-molybdenum dioxide powder.Solid-solid mechanical mix techniques prepare lanthanum-molybdenum oxide powder
Body：(1), nano oxidized state lanthanum is dispersed in solution；(2), nano lanthanum oxide is dispersed into suspension with spray pattern to stirring
Molybdenum dioxide sprinkling under state；(3), step (2) molybdenum dioxide-lanthana-water material stirring is prepared to dry；(4),
The molybdenum dioxide of step (3) preparation-lanthana mixture is crushed, sieving；(5), it by the screenings mixing of step (4), obtains
To lanthana-molybdenum dioxide powder.
Obviously, titanium dioxide is prepared using liquid-solid mechanical mix techniques or solid-solid mechanical mix techniques and molybdenum trioxide is multiple
When closing powder, the mutual diffusion kinetics of titanium dioxide-molybdenum trioxide are insufficient, cause the powder body material uniformity of preparation poor.Tool
The body analysis of causes is as follows：One, titanium dioxide and molybdenum trioxide mechanical mixture lack diffusion motion between molecule rank, cause two
Titanium oxide cannot be uniformly distributed between each other with molybdenum trioxide；Secondly, mechanical mixture when titanium dioxide and molybdenum trioxide exist compared with
Big particle steric hindrance further increases the inhomogeneities that titanium dioxide and molybdenum trioxide are mutually distributed；Third, mechanical mixing operations
Error exacerbates the inhomogeneities that titanium dioxide and molybdenum trioxide are mutually distributed.
It is therefore desirable to develop, a kind of mutual diffusion kinetics of titanium dioxide-molybdenum trioxide are abundant, and titanium dioxide is in molybdenum trioxide
It is evenly distributed in matrix, the preparation method of the titanium dioxide of good product consistency and molybdenum trioxide composite granule.
Summary of the invention
The object of the present invention is to provide the preparation methods of a kind of titanium dioxide and molybdenum trioxide composite granule, provide one kind
It is evenly distributed, the preparation method of the titanium dioxide of good product consistency and molybdenum trioxide composite granule.
The technical scheme adopted by the invention is that the preparation method of a kind of titanium dioxide and molybdenum trioxide composite granule, tool
Body includes the following steps：
Step 1 prepares a water plant acid titanyl ammonium salt solution：Deionized water is added into beaker, continuously adds a water titanium oxalate
Oxygen ammonium, stirring are dissolved completely in a water plant acid titanyl ammonium in deionized water, obtain a water plant acid titanyl ammonium salt solution；
Step 2 prepares ammonium molybdate solution：Ammonium hydroxide is weighed respectively and deionized water is added in same beaker, and beaker is put
It sets on electric heating cover and stirs, continuously add molybdenum trioxide, start electricity consumption heating mantle heats later, heat and stir MoO3-
H2O-NH4OH mixture is completely dissolved molybdenum trioxide to clarification, obtains ammonium molybdate solution；
Step 3, preparation one water plant acid titanyl ammonium-ammonium molybdate solution：The molybdic acid is added in one water plant acid titanyl ammonium salt solution
In ammonium salt solution, 1h-3h is stirred under the conditions of 65 DEG C -90 DEG C, obtains a water plant acid titanyl ammonium-ammonium molybdate solution；
Step 4, preparation one water plant acid titanyl ammonium-ammonium molybdate composite granule：By a water plant acid titanyl ammonium-ammonium molybdate solution into
The spraying dehydration of row, obtains a water plant acid titanyl ammonium-ammonium molybdate composite granule；
Step 5, a water plant acid titanyl ammonium-ammonium molybdate composite granule for preparing certain particle size：By a water plant acid titanyl ammonium-molybdenum
Sour ammonium composite granule is crushed with high speed disintegrator, then sieves smashed water plant acid titanyl ammonium-ammonium molybdate with sieve
Composite granule, under sieving is a water plant acid titanyl ammonium-ammonium molybdate composite granule of certain particle size；
A water plant acid titanyl ammonium-ammonium molybdate composite granule of certain particle size is put into stainless steel material boat by step 6, finally
Stainless steel material boat is put into heating furnace and is heated, titanium dioxide and molybdenum trioxide composite granule are obtained.
The features of the present invention also characterized in that：
The quality of a water plant acid titanyl ammonium is 0.0412-16.4609g in step 1, and the quality of deionized water is 50-550g.
Ammonium hydroxide and the mass ratio of deionized water are 1 in step 2:1-1:3, molybdenum trioxide and deionized water quality ratio are 1:1-
1:3, it is 0.0041-1.6461% that a water plant acid titanyl ammonium, which accounts for molybdenum trioxide mass percent,.
It is stirred when being stirred in step 2 using mechanical stirring device, mixing speed 280-500r/min, heating temperature is
65-85℃。
It is stirred when being stirred in step 3 using mechanical stirring device, mixing speed control is 280-500r/min.
Spraying dehydration is carried out using spray drying tower in step 4, the spray drying tower intake air temperature is 210-
260 DEG C, air outlet temperature is 115-150 DEG C, and the spray drying tower atomizer rotating speed is 0.5 × 104-2.2×104r/min。
The revolving speed of step 5 high speed pulverizer is 0.5 × 104-2.0×104R/min, sieve sieve mesh number are 80-160
Mesh.
A water plant acid titanyl ammonium-ammonium molybdate composite granule thickness of the certain particle size in stainless steel material boat is put into step 6
Degree is 0.5-1.2cm.
Temperature levels direction distribution gradient in step 6 in heating furnace, is followed successively by 350 DEG C -360 DEG C, 410 DEG C -420
DEG C, 470 DEG C -480 DEG C, 450 DEG C -460 DEG C, the stainless steel material boat in heating furnace heating time be 3-5h.
The beneficial effects of the invention are as follows：A kind of preparation method of titanium dioxide and molybdenum trioxide composite granule of the present invention, grass
Sour titanyl ammonium, ammonium molybdate realize the other diffusion motion of molecular level in water-ammonia system, realize the mixing of molecule rank, and liquid-solid
Or solid-solid mechanical mixture is compared, mixed power tends to be infinitely great, and mixing resistance tends to be infinitely small, therefore the titanium dioxide prepared
Titanium-molybdenum trioxide powder uniformity coefficient realizes the raising of matter, ensure that the spectrum standard as measurement molybdenum trioxide Ti content
Molybdenum trioxide sample homogeneity.
Specific embodiment
The present invention is described in detail With reference to embodiment.
A kind of preparation method of titanium dioxide and molybdenum trioxide composite granule of the present invention, specifically comprises the following steps：
Deionized water is added into beaker for step 1, continuously adds a water plant acid titanyl ammonium, and stirring makes a water plant acid titanyl
Ammonium is dissolved completely in deionized water, obtains a water plant acid titanyl ammonium salt solution, wherein a water plant acid titanyl ammonium and deionized water
Mass ratio is 1：3-1：13000.
Step 2 weighs ammonium hydroxide and deionized water is added in beaker respectively, and beaker is placed on electric heating cover and is stirred
It mixes, continuously adds molybdenum trioxide, start electricity consumption heating mantle heats later, heat and continue to stir MoO3-H2O-NH4OH mixture,
It is completely dissolved molybdenum trioxide to clarification, obtains ammonium molybdate solution, wherein ammonium hydroxide and the mass ratio of deionized water are 1:1-1:3,
Molybdenum trioxide and deionized water quality ratio are 1:1-1:3, it is 0.0041- that a water plant acid titanyl ammonium, which accounts for molybdenum trioxide mass percent,
1.6461%, when stirring, is stirred using mechanical stirring device, mixing speed 280-500r/min, and heating temperature is 65-85 DEG C；
The water plant acid titanyl ammonium salt solution is added in the ammonium molybdate solution step 3, under the conditions of 65 DEG C -90 DEG C
1h-3h is stirred, obtains a water plant acid titanyl ammonium-ammonium molybdate solution, when stirring is stirred using mechanical stirring device, mixing speed control
It is made as 280-500r/min；
Step 4 carries out spraying dehydration to a water plant acid titanyl ammonium-ammonium molybdate solution with spray drying tower, obtains a water plant
Sour titanyl ammonium-ammonium molybdate compound, spray drying tower intake air temperature are 210-260 DEG C, and air outlet temperature is 115-150 DEG C,
Spray drying tower atomizer rotating speed is 0.5 × 104-2.2×104r/min；
Step 5 crushes the water plant acid titanyl ammonium-ammonium molybdate compound with high speed disintegrator, then with sieve
Son sieves smashed water plant acid titanyl ammonium-ammonium molybdate compound, and under sieving is that a water plant acid titanyl ammonium-ammonium molybdate is compound
Powder, wherein the revolving speed of high speed disintegrator is 0.5 × 104-2.0×104R/min, sieve sieve mesh number are 80-160 mesh；
One water plant acid titanyl ammonium-ammonium molybdate composite granule is put into stainless steel material boat by step 6, finally by stainless steel material
Boat is put into the heating furnace of temperature distribution gradient and heats 3-5h, obtains titanium dioxide and molybdenum trioxide composite granule, stainless steel
Expect temperature levels direction of a water plant acid titanyl ammonium-ammonium molybdate composite granule in boat with a thickness of 0.5-1.2cm, in heating furnace
Distribution gradient is followed successively by 350 DEG C -360 DEG C, 410 DEG C -420 DEG C, 470 DEG C -480 DEG C, 450 DEG C -460 DEG C.
Embodiment 1
Deionized water 50g is added into beaker for step 1, continuously adds a water plant acid titanyl ammonium 0.0412g, uses glass bar
Stirring is dissolved completely in a water plant acid titanyl ammonium in deionized water, obtains a water plant acid titanyl ammonium salt solution；
Step 2 weighs 1000g ammonium hydroxide and 1000g deionized water is added in same beaker respectively, then places beaker
On electric heating cover and mechanical stirring, mixing speed 280r/min continuously add 1000g molybdenum trioxide, start electricity consumption later
Heating mantle heats heat and stir MoO3-H2O-NH4OH mixture is completely dissolved molybdenum trioxide to clarification, obtains to 65 DEG C
Ammonium molybdate solution；
A water plant acid titanyl ammonium salt solution is added in ammonium molybdate solution step 3, stirs 1h under the conditions of 65 DEG C, obtains one
Water plant acid titanyl ammonium-ammonium molybdate solution；
Step 4 carries out spraying dehydration to a water plant acid titanyl ammonium-ammonium molybdate solution with spray drying tower, will be spray-dried
The control of tower intake air temperature is 210 DEG C, and air outlet temperature control is 115 DEG C, the control of spray drying tower atomizer rotating speed for 0.5 ×
104R/min obtains a water plant acid titanyl ammonium-ammonium molybdate compound；
Step 5 crushes a water plant acid titanyl ammonium-ammonium molybdate compound with high speed disintegrator, and high speed disintegrator turns
Speed control is 1.9 × 104r/min；Secondly smashed water plant acid titanyl ammonium-ammonium molybdate is sieved with the sieve of certain 160 mesh
Compound obtains 160 mesh screenings, as a water plant acid titanyl ammonium-ammonium molybdate composite granule；
160 purpose, one water plant acid titanyl ammonium-ammonium molybdate composite granule is put into stainless steel material boat by step 6, water plant acid
Titanyl ammonium-ammonium molybdate composite granule is put into temperature horizontal direction distribution gradient with a thickness of 0.5cm, by stainless steel material boat
And be followed successively by 350 DEG C -360 DEG C, 410 DEG C -420 DEG C, 470 DEG C -480 DEG C, heat 3h in 450 DEG C -460 DEG C of heating furnace, obtain
To titanium dioxide and molybdenum trioxide composite granule.
Embodiment 2
Deionized water 100g is added into beaker for step 1, continuously adds a water plant acid titanyl ammonium 0.9936g, uses glass bar
Stirring is dissolved completely in a water plant acid titanyl ammonium in deionized water, obtains a water plant acid titanyl ammonium salt solution；
Step 2 weighs 1000g ammonium hydroxide and 2500g deionized water is added in beaker respectively, and beaker is then placed on electricity
In heating mantle and mechanical stirring, mixing speed 460r/min continuously add 1000g molybdenum trioxide, start to use electric heating later
Set heating, heats and stirs MoO3-H2O-NH4OH mixture is completely dissolved molybdenum trioxide to clarification, obtains molybdic acid to 79 DEG C
Ammonium salt solution；
The water plant acid titanyl ammonium salt solution is added in the ammonium molybdate solution step 3, stirs under the conditions of 86 DEG C
3h obtains a water plant acid titanyl ammonium-ammonium molybdate solution；
Step 4 carries out spraying dehydration to a water plant acid titanyl ammonium-ammonium molybdate solution with spray drying tower, will be spray-dried
The control of tower intake air temperature is 239 DEG C, and air outlet temperature control is 136 DEG C, the control of spray drying tower atomizer rotating speed for 2.0 ×
104R/min obtains a water plant acid titanyl ammonium-ammonium molybdate compound；
Step 5 crushes a water plant acid titanyl ammonium-ammonium molybdate compound with high speed disintegrator, and high speed disintegrator turns
Speed control is 1.9 × 104r/min；Secondly smashed water plant acid titanyl ammonium-ammonium molybdate is sieved with the sieve of certain 160 mesh
Compound obtains 160 mesh screenings, as a water plant acid titanyl ammonium-ammonium molybdate composite granule；
160 purpose, one water plant acid titanyl ammonium-ammonium molybdate composite granule is put into stainless steel material boat by step 6, water plant acid
Titanyl ammonium-ammonium molybdate composite granule is put into temperature horizontal direction distribution gradient with a thickness of 0.5cm, by stainless steel material boat
And be followed successively by 350 DEG C -360 DEG C, 410 DEG C -420 DEG C, 470 DEG C -480 DEG C, heat 3h in 450 DEG C -460 DEG C of heating furnace, obtain
To titanium dioxide and molybdenum trioxide composite granule.
Embodiment 3
Deionized water 350g is added into beaker for step 1, continuously adds a water plant acid titanyl ammonium 4.5706g, uses glass bar
Stirring is dissolved completely in a water plant acid titanyl ammonium in deionized water, obtains a water plant acid titanyl ammonium salt solution；
Step 2 weighs 1000g ammonium hydroxide and 1500g deionized water is added in beaker respectively, and beaker is then placed on electricity
In heating mantle and mechanical stirring, mixing speed 360r/min continuously add 1000g molybdenum trioxide, start to use electric heating later
Set heating, heats and stirs MoO3-H2O-NH4OH mixture is completely dissolved molybdenum trioxide to clarification, obtains molybdic acid to 70 DEG C
Ammonium salt solution；
A water plant acid titanyl ammonium salt solution is added in ammonium molybdate solution step 3, stirs 1.5h under the conditions of 70 DEG C, obtains
One water plant acid titanyl ammonium-ammonium molybdate solution；
Step 4 carries out spraying dehydration to a water plant acid titanyl ammonium-ammonium molybdate solution with spray drying tower, will be spray-dried
The control of tower intake air temperature is 230 DEG C, and air outlet temperature control is 120 DEG C, the control of spray drying tower atomizer rotating speed for 1.3 ×
104R/min obtains a water plant acid titanyl ammonium-ammonium molybdate compound；
Step 5 crushes a water plant acid titanyl ammonium-ammonium molybdate compound with high speed disintegrator, and high speed disintegrator turns
Speed control is 1.5 × 104r/min；Secondly smashed water plant acid titanyl ammonium-ammonium molybdate is sieved with the sieve of certain 120 mesh
Compound obtains 120 mesh screenings, as a water plant acid titanyl ammonium-ammonium molybdate composite granule；
120 purpose, one water plant acid titanyl ammonium-ammonium molybdate composite granule is put into stainless steel material boat by step 6, water plant acid
Titanyl ammonium-ammonium molybdate composite granule is put into temperature horizontal direction distribution gradient with a thickness of 0.8cm, by stainless steel material boat
And be followed successively by 350 DEG C -360 DEG C, 410 DEG C -420 DEG C, 470 DEG C -480 DEG C, heat 3.5h in 450 DEG C -460 DEG C of heating furnace,
Obtain titanium dioxide and molybdenum trioxide composite granule.
Embodiment 4
Deionized water 400g is added into beaker for step 1, continuously adds a water plant acid titanyl ammonium 10.3572g, uses glass
Stick stirring is dissolved completely in a water plant acid titanyl ammonium in deionized water, obtains a water plant acid titanyl ammonium salt solution；
Step 2 weighs 1000g ammonium hydroxide and 2000g deionized water is added in beaker respectively, and beaker is then placed on electricity
In heating mantle and mechanical stirring, mixing speed 400r/min continuously add 1000g molybdenum trioxide, start to use electric heating later
Set heating, heats and stirs MoO3-H2O-NH4OH mixture is completely dissolved molybdenum trioxide to clarification, obtains molybdic acid to 76 DEG C
Ammonium salt solution；
A water plant acid titanyl ammonium salt solution is added in ammonium molybdate solution step 3, stirs 1.5h under the conditions of 83 DEG C, obtains
One water plant acid titanyl ammonium-ammonium molybdate solution；
Step 4 carries out spraying dehydration to a water plant acid titanyl ammonium-ammonium molybdate solution with spray drying tower, will be spray-dried
The control of tower intake air temperature is 235 DEG C, and air outlet temperature control is 121 DEG C, the control of spray drying tower atomizer rotating speed for 1.6 ×
104R/min obtains a water plant acid titanyl ammonium-ammonium molybdate compound；
Step 5 crushes a water plant acid titanyl ammonium-ammonium molybdate compound with high speed disintegrator, and high speed disintegrator turns
Speed control is 1.5 × 104r/min；Secondly smashed water plant acid titanyl ammonium-ammonium molybdate is sieved with the sieve of certain 120 mesh
Compound obtains 120 mesh screenings, as a water plant acid titanyl ammonium-ammonium molybdate composite granule；
120 purpose, one water plant acid titanyl ammonium-ammonium molybdate composite granule is put into stainless steel material boat by step 6, water plant acid
Titanyl ammonium-ammonium molybdate composite granule is put into temperature horizontal direction distribution gradient with a thickness of 1.0cm, by stainless steel material boat
And be followed successively by 350 DEG C -360 DEG C, 410 DEG C -420 DEG C, 470 DEG C -480 DEG C, heat 4h in 450 DEG C -460 DEG C of heating furnace, obtain
To titanium dioxide and molybdenum trioxide composite granule.
Embodiment 5
Deionized water 500g is added into beaker for step 1, continuously adds a water plant acid titanyl ammonium 16.4609g g, uses glass
The stirring of glass stick is dissolved completely in a water plant acid titanyl ammonium in deionized water, obtains a water plant acid titanyl ammonium salt solution；
Step 2 weighs 1000g ammonium hydroxide and 3000g deionized water is added in beaker respectively, and beaker is then placed on electricity
In heating mantle and mechanical stirring, mixing speed 500r/min continuously add 1000g molybdenum trioxide, start to use electric heating later
Set heating, heats and stirs MoO3-H2O-NH4OH mixture is completely dissolved molybdenum trioxide to clarification, obtains molybdic acid to 85 DEG C
Ammonium salt solution；
A water plant acid titanyl ammonium salt solution is added in ammonium molybdate solution step 3, stirs 3h under the conditions of 90 DEG C, obtains one
Water plant acid titanyl ammonium-ammonium molybdate solution；
Step 4 carries out spraying dehydration to a water plant acid titanyl ammonium-ammonium molybdate solution with spray drying tower, will be spray-dried
The control of tower intake air temperature is 255 DEG C, and air outlet temperature control is 148 DEG C, the control of spray drying tower atomizer rotating speed for 2.1 ×
104R/min obtains a water plant acid titanyl ammonium-ammonium molybdate compound；
Step 5 crushes a water plant acid titanyl ammonium-ammonium molybdate compound with high speed disintegrator, and high speed disintegrator turns
Speed control is 2.0 × 104r/min；Secondly it is multiple smashed water plant acid titanyl ammonium-ammonium molybdate to be sieved with the sieve of certain 80 mesh
Object is closed, 80 mesh screenings, as a water plant acid titanyl ammonium-ammonium molybdate composite granule are obtained；
80 purpose, one water plant acid titanyl ammonium-ammonium molybdate composite granule is put into stainless steel material boat by step 6, water plant acid
Titanyl ammonium-ammonium molybdate composite granule is put into temperature horizontal direction distribution gradient with a thickness of 1.2cm, by stainless steel material boat
And be followed successively by 350 DEG C -360 DEG C, 410 DEG C -420 DEG C, 470 DEG C -480 DEG C, heat 5h in 450 DEG C -460 DEG C of heating furnace, obtain
To titanium dioxide and molybdenum trioxide composite granule.
Molybdenum trioxide molybdenum content used in above embodiments 1- embodiment 5 is that 66.53%, one water plant acid titanyl ammonium purity is
98%, reagent ammonium hydroxide purity 25%~28%, titanium dioxide and molybdenum trioxide composite granule metal Ti content 0.1231%, molybdenum contains
Measure content 66.38%.
Claims (9)
1. the preparation method of a kind of titanium dioxide and molybdenum trioxide composite granule, it is characterised in that：Specifically comprise the following steps：
Deionized water is added into beaker for step 1, continuously adds a water plant acid titanyl ammonium, and stirring keeps a water plant acid titanyl ammonium complete
Fully dissolved obtains a water plant acid titanyl ammonium salt solution in deionized water；
Step 2 weighs ammonium hydroxide and deionized water is added in beaker respectively, and beaker is placed on electric heating cover and is stirred, after
It is continuous that molybdenum trioxide is added, start electricity consumption heating mantle heats later, continues to stir MoO3-H2O-NH4OH mixture, makes molybdenum trioxide
It is completely dissolved to clarification, obtains ammonium molybdate solution；
The water plant acid titanyl ammonium salt solution is added in the ammonium molybdate solution step 3, stirs under the conditions of 65 DEG C -90 DEG C
1h-3h obtains a water plant acid titanyl ammonium-ammonium molybdate solution；
The one water plant acid titanyl ammonium-ammonium molybdate solution is carried out spraying dehydration by step 4, obtains a water plant acid titanyl ammonium-molybdic acid
Ammonium compound；
Step 5 crushes the water plant acid titanyl ammonium-ammonium molybdate compound with high speed disintegrator, is then sieved with sieve
Divide smashed water plant acid titanyl ammonium-ammonium molybdate compound, under sieving is a water plant acid titanyl ammonium-ammonium molybdate composite powder
Body；
The one water plant acid titanyl ammonium-ammonium molybdate composite granule is put into stainless steel material boat by step 6, finally will be described stainless
Steel material boat, which is put into heating furnace, to be heated, and titanium dioxide and molybdenum trioxide composite granule are obtained.
2. the preparation method of a kind of titanium dioxide and molybdenum trioxide composite granule according to claim 1, it is characterised in that：
The mass ratio of a water plant acid titanyl ammonium and ionized water is 1 in the step 1：3-1：13000.
3. the preparation method of a kind of titanium dioxide and molybdenum trioxide composite granule according to claim 1, it is characterised in that：
Ammonium hydroxide and the mass ratio of deionized water are 1 in the step 2:1-1:3, molybdenum trioxide and deionized water quality ratio are 1:1-1:3,
It is 0.0041-1.6461% that one water plant acid titanyl ammonium, which accounts for molybdenum trioxide mass percent,.
4. the preparation method of a kind of titanium dioxide and molybdenum trioxide composite granule according to claim 1, it is characterised in that：
It is stirred when being stirred in the step 2 using mechanical stirring device, mixing speed 280-500r/min, heating temperature 65-85
℃。
5. the preparation method of a kind of titanium dioxide and molybdenum trioxide composite granule according to claim 1, it is characterised in that：
It is stirred when being stirred in the step 3 using mechanical stirring device, mixing speed control is 280-500r/min.
6. the preparation method of a kind of titanium dioxide and molybdenum trioxide composite granule according to claim 1, it is characterised in that：
Spraying dehydration is carried out using spray drying tower in the step 4, the spray drying tower intake air temperature is 210-260
DEG C, air outlet temperature is 115-150 DEG C, and the spray drying tower atomizer rotating speed is 0.5 × 104-2.2×104r/min。
7. the preparation method of a kind of titanium dioxide and molybdenum trioxide composite granule according to claim 1, it is characterised in that：
The revolving speed of the step 5 high speed pulverizer is 0.5 × 104-2.0×104R/min, sieve sieve mesh number are 80-160 mesh.
8. the preparation method of a kind of titanium dioxide and molybdenum trioxide composite granule according to claim 1, it is characterised in that：
A water plant acid titanyl ammonium-ammonium molybdate composite granule in stainless steel material boat is put into the step 6 with a thickness of 0.5-1.2cm.
9. the preparation method of a kind of titanium dioxide and molybdenum trioxide composite granule according to claim 1, it is characterised in that：
Temperature levels direction distribution gradient in the step 6 in heating furnace, is followed successively by 350 DEG C -360 DEG C, 410 DEG C -420 DEG C, 470
DEG C -480 DEG C, 450 DEG C -460 DEG C, heating time is 3-5h to the stainless steel material boat in heating furnace.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810618330.5A CN108910951B (en) | 2018-06-15 | 2018-06-15 | Preparation method of titanium dioxide and molybdenum trioxide composite powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810618330.5A CN108910951B (en) | 2018-06-15 | 2018-06-15 | Preparation method of titanium dioxide and molybdenum trioxide composite powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108910951A true CN108910951A (en) | 2018-11-30 |
| CN108910951B CN108910951B (en) | 2020-08-25 |
Family
ID=64420393
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810618330.5A Active CN108910951B (en) | 2018-06-15 | 2018-06-15 | Preparation method of titanium dioxide and molybdenum trioxide composite powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108910951B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111257070A (en) * | 2020-01-17 | 2020-06-09 | 金堆城钼业股份有限公司 | Preparation method of molybdenum trioxide spectrum internal control standard sample |
| CN115446323A (en) * | 2022-09-22 | 2022-12-09 | 西北有色金属研究院 | Method for preparing tungsten-molybdenum powder by using waste target scrap powder of tungsten and molybdenum |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58183946A (en) * | 1982-04-20 | 1983-10-27 | Mitsubishi Heavy Ind Ltd | Denitration catalyst and preparation thereof |
| CN101757907A (en) * | 2008-12-26 | 2010-06-30 | 晶锐瓷业（北京）有限公司 | Titanium dioxide powder containing tungsten for preparing honeycomb SCR DeNOx catalyst and preparation method thereof |
| CN101972647A (en) * | 2010-11-26 | 2011-02-16 | 山东电力研究院 | Titanium-base granular catalyst and preparation method and application thereof |
| CN102745739A (en) * | 2011-04-21 | 2012-10-24 | 苏州科技学院 | Preparation method of oxide nanocrystal solid |
-
2018
- 2018-06-15 CN CN201810618330.5A patent/CN108910951B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58183946A (en) * | 1982-04-20 | 1983-10-27 | Mitsubishi Heavy Ind Ltd | Denitration catalyst and preparation thereof |
| CN101757907A (en) * | 2008-12-26 | 2010-06-30 | 晶锐瓷业（北京）有限公司 | Titanium dioxide powder containing tungsten for preparing honeycomb SCR DeNOx catalyst and preparation method thereof |
| CN101972647A (en) * | 2010-11-26 | 2011-02-16 | 山东电力研究院 | Titanium-base granular catalyst and preparation method and application thereof |
| CN102745739A (en) * | 2011-04-21 | 2012-10-24 | 苏州科技学院 | Preparation method of oxide nanocrystal solid |
Non-Patent Citations (1)
| Title |
|---|
| SHOULI BAI等: "Improvement of TiO2 photocatalytic properties under visible light byWO3/TiO2 and MoO3/TiO2 composites", 《APPLIED SURFACE SCIENCE》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111257070A (en) * | 2020-01-17 | 2020-06-09 | 金堆城钼业股份有限公司 | Preparation method of molybdenum trioxide spectrum internal control standard sample |
| CN111257070B (en) * | 2020-01-17 | 2023-03-10 | 金堆城钼业股份有限公司 | Preparation method of molybdenum trioxide spectrum internal control standard sample |
| CN115446323A (en) * | 2022-09-22 | 2022-12-09 | 西北有色金属研究院 | Method for preparing tungsten-molybdenum powder by using waste target scrap powder of tungsten and molybdenum |
| CN115446323B (en) * | 2022-09-22 | 2024-03-22 | 西北有色金属研究院 | Method for preparing tungsten-molybdenum powder by utilizing waste target scraps of tungsten and molybdenum |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108910951B (en) | 2020-08-25 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| EP2429975B1 (en) | Process for preparing an elemental sulphur-containing fertilizer | |
| CN100463851C (en) | Method for preparing super fine hydrophobic silicon dioxide | |
| CN110951280B (en) | Copper-chromium black toner prepared by solid-phase sintering method promoted by molybdenum oxide and manganese oxide and preparation method thereof | |
| CN108910951A (en) | A kind of preparation method of titanium dioxide and molybdenum trioxide composite granule | |
| CN110323434A (en) | Prepare iron manganese phosphate for lithium-carbon composite method and iron manganese phosphate for lithium-carbon composite | |
| CN214438963U (en) | Ferric phosphate production measurement feeding device | |
| CN102701255A (en) | Method for high-concentration carbonization production of spherical nano calcium carbonate | |
| CN103551201A (en) | Method for preparing copper hydroxyphosphate catalyst | |
| CN109848431B (en) | Preparation method of fine molybdenum powder | |
| CN107902690A (en) | Preparation method of micron-sized tin dioxide | |
| CN105817178B (en) | A kind of atomized molten system and using activity spherical cuprous chloride catalyst made from the system and preparation method thereof | |
| CN108218694A (en) | A kind of preparation method of ultra-fine calcium citrate | |
| CN110422881B (en) | Preparation method of high-activity trimanganese tetroxide | |
| CN108311134A (en) | Diesel vehicle/steamer tail gas SCR denitration titanium tungsten silicon composite powder and preparation method | |
| CN109288035B (en) | Processing method of high-stability lotus seed starch-soybean lecithin compound | |
| CN110183324A (en) | A kind of preparation process of stearate | |
| CN1331817C (en) | Method for producing agricultural granular magnesium sulfate fertilizer | |
| CN106830042A (en) | The method that a kind of utilization Weihe north Ordovician limestone prepares the ultra-fine carbonic acid fine particle calcium carbonate of rhombohedron shape | |
| CN107032413B (en) | The preparation method of iron oxide red | |
| CN105905885A (en) | Preparation method of straw-core carbon material | |
| US4104189A (en) | Curing agent for polysulfide-polymer compositions | |
| CN109894046A (en) | A kind of compound fertilizer's melting mixing system | |
| CN2133358Y (en) | Powder producing device with grinding, mixing, heating and coating functions | |
| CN1277752C (en) | Process for preparing cobaltosic oxide powder by solid-phase catalytic oxidation of cobaltous chloride | |
| CN100502851C (en) | Formula and preparation method for compound ointment containing zinc undecylenate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |