CN105460973B - The method that white carbon/composite titania material is prepared using potassium feldspar - Google Patents
The method that white carbon/composite titania material is prepared using potassium feldspar Download PDFInfo
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- CN105460973B CN105460973B CN201510851578.2A CN201510851578A CN105460973B CN 105460973 B CN105460973 B CN 105460973B CN 201510851578 A CN201510851578 A CN 201510851578A CN 105460973 B CN105460973 B CN 105460973B
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- white carbon
- ammonium
- potassium feldspar
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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05C—NITROGENOUS FERTILISERS
- C05C3/00—Fertilisers containing other salts of ammonia or ammonia itself, e.g. gas liquor
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- Life Sciences & Earth Sciences (AREA)
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Abstract
The method that potassium feldspar prepares white carbon/composite titania material is the present invention relates to the use of, is that raw material prepares SiF using potassium feldspar, ammonium fluoride, the concentrated sulfuric acid4Gas, recycles ammoniacal liquor to the SiF4Gas is absorbed, while to adding titanium tetrachloride in the ammoniacal liquor so that titanium tetrachloride and SiF4Gas can synchronously be hydrolyzed, and the product after hydrolysis is aged, filtering, washing, carry out high-temperature calcination so as to white carbon/composite titania material is obtained after drying.While potassium feldspar resource is made full use of, the white carbon/composite titania material of acquisition is respectively provided with excellent photocatalysis performance, and preparation process is simple to the present invention under ultraviolet light and visible ray, and raw material availability is high.
Description
Technical field
The present invention relates to a kind of preparation method of composite titania material, specifically, relate to using potassium feldspar system
The method of standby white carbon/composite titania material.
Background technology
Titanium dioxide because its have stability it is high, with photo-catalysis function, it is cheap the features such as, be widely used in photocatalysis row
Industry, but actually preparing photocatalysis TiO2When, because of its extremely easy reunion, it is difficult to reclaim and also exist TiO2Photochemical catalyst is certainly
The not high defect of right light utilization efficiency, constrains TiO2The catalytic efficiency of photochemical catalyst.Current result of the above problems is usual
It is by the TiO2Photocatalyst on suitable carrier material, to improve the photocatalysis rate of titanium dioxide, preparation technology
Cumbersome, raw material availability is low.
Precipitated silica is a kind of amorphous silica powder body material with waterglass as main material production, with than
The features such as surface area is big, porosity is high, aperture is small, chemical stability is good is a kind of with performance advantage and cost advantage
TiO2Carrier material；On the other hand, the potash feldspar ore reserves of China extremely enrich, potassium feldspar contain abundant potassium, aluminium, silicon etc. into
Point, therefore, it can by preparing white carbon to potassium feldspar comprehensive exploitation, and silicon tetrachloride etc. is synchronously added in preparation process
Raw material is directly obtained white carbon/composite titania material by reaction.
The content of the invention
The technical solution adopted in the present invention is：The method that white carbon/composite titania material is prepared using potassium feldspar,
Specifically include following steps：
Step one, potassium feldspar, ammonium fluoride, the concentrated sulfuric acid be added in reactor successively, it is at 200 DEG C~300 DEG C and spontaneous
Reacted under pressure, generated gas and solid residue, its reaction principle is：
NH4F =HF↑ + NH3↑,
2K[AlSi3O8] + 24HF + 4H2SO4 = K2SO4 + Al2(SO4)3 + 6SiF4+ 16H2O,
Wherein, potassium feldspar, ammonium fluoride, the mass ratio of the concentrated sulfuric acid are 1：3~3.5：3.5~4；The concentrated sulfuric acid is by mass fraction
98% concentrated sulfuric acid is calculated；
Step 2, in the case where temperature is 5 DEG C~10 DEG C and condition of negative pressure, be passed through in the ammoniacal liquor for mass fraction being 20%~30%
The gas, while to adding titanium tetrachloride in the ammoniacal liquor, and the gas and the titanium tetrachloride are made by magnetic agitation
There is hydrolysis generation turbid solution simultaneously, the turbid solution is aged, filtering, washing, obtain compound after drying, its reaction
Principle is mainly：
TiCl4+ 2H2O=TiO2↓+4HCl,
3SiF4 + 2H2O = 2H2SiF6 + SiO2↓,
H2SiF6 +6NH4OH = 6NH4F + SiO2↓ + 4H2O,
NH4OH + HCl = NH4Cl + H2O ；
Step 3, by the compound temperature be 500 DEG C~1100 DEG C at carry out the h of high-temperature calcination 6~8, be cooled to room
White carbon/composite titania material is obtained after temperature.
Based on above-mentioned, the step one be additionally included in temperature for used under the conditions of 90 DEG C~110 DEG C mass fraction for 8%~
10% sulfuric acid solution leaches the solid residue, and leaching liquid is obtained, to addition ammoniacal liquor regulation pH=8~10 in the leaching liquid,
By obtaining ammonium-potassium sulfate filtrate and aluminum hydroxide precipitation after filtering, then by the ammonium-potassium sulfate filtrate by being concentrated in vacuo to
Saturation, separates out ammonium-potassium sulfate crystal；Finally by slurry-spraying pelletizing, it is drying to obtain binary compound fertilizer ammonium-potassium sulfate.
Based on above-mentioned, the turbid solution in the step 2 is aged, obtain after filtering and contain ammonium fluoride, the filter of ammonium chloride
Liquid, the filtrate obtains ammonium fluoride and can be heated as the ammonium chloride crystals particle of nitrogenous fertilizer, the ammonium fluoride through evaporative crystallization
Decomposing generation hydrogen fluoride and ammonia can recycle.
Based on above-mentioned, the step 3 also includes：The compound is passed through in spraying reaction tower in atomization temperature first
To carry out 10~35s of atomization under the conditions of 70 DEG C~95 DEG C, atomizing particle size is 5~100 microns, atomized after recovered drying
Grain, then carries out the h of high-temperature calcination 6~8 again by the atomizing particle under the conditions of temperature is for 500 DEG C~1100 DEG C, is cooled to room
White carbon/composite titania material is obtained after temperature.
The present invention has prominent substantive distinguishing features progressive with significant compared with the prior art, specifically,
Ammonium fluoride, potassium feldspar decomposition are produced SiF by the present invention first4Gas, recycles ammoniacal liquor to the SiF4Gas is carried out
Hydrolysis is absorbed, titanium tetrachloride is added in hydrolytic process, the product after hydrolysis is aged, filtering, washing, carry out high temperature after drying and forge
Burn so as to white carbon/composite titania material is obtained.
Preparation process process is simple of the present invention, reaction condition enter water-filling gently, to equipment than relatively low to titanium tetrachloride
In solution preocess, SiF is contained because being passed through4Gas, not only play a part of reactant, the effect of stirring is also acted, with same
When in the presence of magnetic agitation so that the composite of preparation is more uniform, it is to avoid the agglomeration of titanium dioxide, improves
Its photocatalysis efficiency.Further, in the preparation process intermediate product can be carried by recycling generation byproduct
The utilization rate of potassium feldspar high.
Specific embodiment
Below by specific embodiment, technical scheme is described in further detail.
Embodiment 1
The present embodiment provides a kind of method that utilization potassium feldspar prepares white carbon/composite titania material, specific steps
Including：
Step one, potassium feldspar, ammonium fluoride, the concentrated sulfuric acid be added in converter reactor successively, in 200 DEG C and self-generated pressure
Under reacted, generate gas and solid residue, its reaction principle is：
NH4F =2HF↑ + NH3↑,
2K[AlSi3O8] + 24HF + 4H2SO4 = K2SO4 + Al2(SO4)3 + 6SiF4+ 16H2O,
Wherein, potassium feldspar, ammonium fluoride, the mass ratio of the concentrated sulfuric acid are 1：3.5：4；The concentrated sulfuric acid for mass fraction be 98% it is dense
Sulfuric acid；
Step 2, in the case where temperature is 10 DEG C and condition of negative pressure, in absorption column of gas to mass fraction be 25% ammoniacal liquor in
The gas of step one generation is passed through, while to adding titanium tetrachloride in the ammoniacal liquor, and the gas is made by magnetic agitation
There is hydrolysis generation turbid solution simultaneously in body and the titanium tetrachloride, the turbid solution is aged, filtering, washing, after drying
Compound is obtained, its reaction principle is mainly：
TiCl4+ 2H2O=TiO2↓+4HCl,
3SiF4 + 2H2O = 2H2SiF6 + SiO2↓,
H2SiF6 +6NH4OH = 6NH4F + SiO2↓ + 4H2O,
NH4OH + HCl = NH4Cl + H2O ；
Step 3, the compound is positioned in calcining furnace be 1100 DEG C in temperature at carry out the h of high-temperature calcination 6, cool down
White carbon/composite titania material is obtained after to room temperature.
Embodiment 2
The present embodiment provides a kind of method that utilization potassium feldspar prepares white carbon/composite titania material, specific steps
Roughly the same with embodiment 1, difference is：
Step one, potassium feldspar, ammonium fluoride, the concentrated sulfuric acid be added in converter reactor successively, in 250 DEG C and self-generated pressure
Under reacted, generate gas and solid residue, its reaction principle is：
NH4F =2HF↑ + NH3↑,
2K[AlSi3O8] + 24HF + 4H2SO4 = K2SO4 + Al2(SO4)3 + 6SiF4+ 16H2O,
Wherein, potassium feldspar, ammonium fluoride, the mass ratio of the concentrated sulfuric acid are 1：3.5：4；The concentrated sulfuric acid for mass fraction be 98% it is dense
Sulfuric acid.At the solid residue is 110 DEG C in temperature, after being leached through the sulfuric acid solution that mass fraction is 10%, in leaching liquid
It is 10 to add ammoniacal liquor to adjust the pH of the leaching liquid, ammonium-potassium sulfate filtrate and aluminum hydroxide precipitation is obtained after filtering, then by institute
Ammonium-potassium sulfate filtrate is stated by being concentrated in vacuo to saturation, ammonium-potassium sulfate crystal is separated out；And by slurry-spraying pelletizing, be drying to obtain two
Component composite fertilizer ammonium-potassium sulfate；
Step 2, in the case where temperature is 5 DEG C and condition of negative pressure, in absorption column of gas to mass fraction be 20% ammoniacal liquor in
The gas of step one generation is passed through, while to adding titanium tetrachloride in the ammoniacal liquor, and the gas is made by magnetic agitation
There is hydrolysis generation turbid solution simultaneously in body and the titanium tetrachloride, the turbid solution is aged, filtering, washing, after drying
Obtain compound.Turbid solution filtrate after filtering is obtained ammonium fluoride and can be as the ammonium chloride of nitrogenous fertilizer through evaporative crystallization
Crystalline particle, the ammonium fluoride is thermally decomposed to generate hydrogen fluoride and ammonia and can be recycled.
Embodiment 3
The present embodiment provides a kind of method that utilization potassium feldspar prepares white carbon/composite titania material, specific steps
Roughly the same with embodiment 1, difference is：
Step 3, the compound is passed through in spraying reaction tower and carries out atomization 35s, it is 95 DEG C, mist to control atomization temperature
It is 5~100 microns to change particle diameter, and then be positioned over the atomizing particle in calcining furnace by atomized particle after recovered drying
High-temperature calcination 6h is carried out at being 1000 DEG C in temperature, is obtained with white carbon/composite titania material.
Finally it should be noted that：The above embodiments are merely illustrative of the technical solutions of the present invention rather than its limitations；To the greatest extent
Pipe has been described in detail with reference to preferred embodiment to the present invention, and those of ordinary skill in the art should be understood：Still
Specific embodiment of the invention can be modified or equivalent is carried out to some technical characteristics；Without deviating from this hair
The spirit of bright technical scheme, it all should cover in the middle of claimed technical scheme scope of the invention.
Claims (3)
1. the method that white carbon/composite titania material is prepared using potassium feldspar, specifically includes following steps：
Step one, potassium feldspar, ammonium fluoride, the concentrated sulfuric acid be added in reactor successively, in 200 DEG C~300 DEG C and self-generated pressure
Under reacted, generate gas and solid residue, wherein, potassium feldspar, ammonium fluoride, the concentrated sulfuric acid mass ratio be 1：3~3.5：3.5
~4；
Step 2, in the case where temperature is 5 DEG C~10 DEG C and condition of negative pressure, be passed through in the ammoniacal liquor for mass fraction being 20%~30% described
The gas of step one generation, while to adding titanium tetrachloride in the ammoniacal liquor, and by magnetic agitation make the gas and
There is hydrolysis generation turbid solution in the titanium tetrachloride, the turbid solution is aged, filtering, washing, obtain after drying simultaneously
Compound；
Step 3, first by the compound be passed through in spraying reaction tower be 70 DEG C~95 DEG C in atomization temperature under the conditions of carry out mist
Change 10~35s, atomizing particle size is 5~100 microns, and then atomized particle after recovered drying exists the atomizing particle
Temperature is obtained white carbon/titanium dioxide to carry out the h of high-temperature calcination 6~8 again under the conditions of 500 DEG C~1100 DEG C after being cooled to room temperature
Composite.
2. the method that utilization potassium feldspar according to claim 1 prepares white carbon/composite titania material, its feature exists
In it also includes：Mass fraction is used to leach institute for 8%~10% sulfuric acid solution under the conditions of being 90 DEG C~110 DEG C in temperature
Solid residue is stated, leaching liquid is obtained, to ammoniacal liquor regulation pH=8~10 are added in the leaching liquid, by obtaining ammonium sulfate after filtering
Potassium filtrate and aluminum hydroxide precipitation, then make ammonium-potassium sulfate crystal by the ammonium-potassium sulfate filtrate by being concentrated in vacuo to saturation
Separate out；Finally by slurry-spraying pelletizing, it is drying to obtain binary compound fertilizer ammonium-potassium sulfate.
3. the method that utilization potassium feldspar according to claim 1 prepares white carbon/composite titania material, its feature exists
In the turbid solution in the step 2 is aged, obtain after filtering and contain ammonium fluoride, the filtrate of ammonium chloride, the filtrate warp
Evaporative crystallization obtains ammonium fluoride and the ammonium chloride crystals particle as nitrogenous fertilizer, and the ammonium fluoride is thermally decomposed to generate hydrogen fluoride and ammonia
Gas so that the ammonium fluoride is recycled.
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| CN102039117B (en) * | 2009-10-15 | 2012-08-08 | 中国矿业大学(北京) | Method for preparing loaded nano TiO2 composite material by using precipitated white carbon black as carrier |
| CN103172074B (en) * | 2013-01-17 | 2014-11-26 | 洛阳氟钾科技有限公司 | Process for decomposing potassium feldspar by adopting low-temperature semidry method for comprehensive utilization |
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