CN108640150A - A kind of preparation method of dioxide for denitration through use of titanium additional hydrolyzing seed crystal - Google Patents
A kind of preparation method of dioxide for denitration through use of titanium additional hydrolyzing seed crystal Download PDFInfo
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- CN108640150A CN108640150A CN201810589555.2A CN201810589555A CN108640150A CN 108640150 A CN108640150 A CN 108640150A CN 201810589555 A CN201810589555 A CN 201810589555A CN 108640150 A CN108640150 A CN 108640150A
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- Prior art keywords
- titanium
- denitration
- dioxide
- sodium hydroxide
- hydroxide solution
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- 239000013078 crystal Substances 0.000 title claims abstract description 46
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 239000010936 titanium Substances 0.000 title claims abstract description 43
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 230000003301 hydrolyzing effect Effects 0.000 title claims abstract description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 93
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 75
- 239000007788 liquid Substances 0.000 claims abstract description 30
- 238000010792 warming Methods 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 150000001875 compounds Chemical class 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 239000000126 substance Substances 0.000 claims description 2
- 239000004408 titanium dioxide Substances 0.000 abstract description 24
- 238000000034 method Methods 0.000 abstract description 15
- 230000007062 hydrolysis Effects 0.000 abstract description 14
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 14
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 8
- 239000003054 catalyst Substances 0.000 abstract description 6
- 239000002994 raw material Substances 0.000 abstract description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 abstract description 4
- 238000001125 extrusion Methods 0.000 abstract description 4
- 235000010215 titanium dioxide Nutrition 0.000 description 26
- 238000009826 distribution Methods 0.000 description 4
- 238000001723 curing Methods 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 3
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 229910000349 titanium oxysulfate Inorganic materials 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 229910003074 TiCl4 Inorganic materials 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- XTQHKBHJIVJGKJ-UHFFFAOYSA-N sulfur monoxide Chemical compound S=O XTQHKBHJIVJGKJ-UHFFFAOYSA-N 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium(II) oxide Chemical compound [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/64—Pore diameter
- B01J35/647—2-50 nm
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of preparation methods of dioxide for denitration through use of titanium additional hydrolyzing seed crystal, include the following steps:Step1, the technical grade titanium liquid for meeting titanium liquid index is taken, is warming up to 70~90 DEG C;Then Step2, the sodium hydroxide solution that compound concentration is 2.0~6.0mol/L are warming up to 70~90 DEG C;Step3, the titanium liquid of Step1 is added in the sodium hydroxide solution obtained in Step2, after stirring evenly, is heated to 90~120 DEG C, then kept the temperature 0~90min and cured;Step4, crystal seed stability reach 150ml hereinafter, reaction is hydrolyzed, and obtain crystal seed.Raw material of the present invention is the black titanium liquid of Production By Sulfuric Acid Process, low for equipment requirements, and the hydrolysis crystal seed activity prepared is high, and the denitration titanium dioxide produced is suitable for the extrusion of denitrating catalyst production, forming process.
Description
Technical field
The present invention relates to titanium white production technical fields, more particularly to a kind of dioxide for denitration through use of titanium additional hydrolyzing seed crystal
Preparation method.
Background technology
In recent years, China is invaded by haze, acid rain often so that country greatly increases environmentally friendly dynamics, especially
It is the discharge about nitrogen oxides, oxysulfide, all coal-burning power plants, coal-burning boiler, coal chemical industry is strictly required in National Development and Reform Committee
Device installs desulphurization denitration and dust removal installation.Meanwhile accelerating to put into effect the coal-fired utilities such as thermal power generation, coking, building materials, coal-burning boiler
Pollutant emission new standard adds pollutant emission index, further stringent pollutant emission limit.In addition, also reinforcing desulfurization
The environmental protection facilities rolling inspection such as denitration and dedusting, it is ensured that related environmental protection facility normal operation plays the role of to have, denitration as a result,
The market potential of titanium dioxide gradually highlights.
Since denitration titanium dioxide quality requirement is higher, raw material are fixed against import more, and Cost Control is simultaneously unstable,
And denitration titanium dioxide technology domestic at present is still immature, the denitration produced is irregular with titanium dioxide actual mass, therefore,
The technique of current denitration titanium dioxide is improved, application performance gesture of the denitration titanium dioxide in catalyst preparation process is improved
It must go.
Chinese patent 200610039318 discloses a kind of preparation method for producing the hydrolysis crystal seed of titanium dioxide, should
Method is mixed with crystal seed by sodium hydroxide and titanyl sulfate solution, carries out plus seed hydrolysis, although shortening the system of crystal seed
The standby time, the concentration of previous process concentrated vitriol oxygen titanium solution is reduced, improves the pigment and optical property of titanium dioxide, but its
The aperture of the titanium dioxide of preparation optimizes only in 5~10nm or so for pigment titanium white performance, is not suitable for denitrating catalyst use
The preparation of titanium dioxide.
Chinese patent 201010202414.4 discloses a kind of method preparing titanium dioxide hydrolysis crystal seed, and this method passes through
TiCl4As titanium source, crystal seed preparation is carried out, this method is although simple for process, low for equipment requirements, and activity of crystal seed is stablized, but its
Material purity requires crystal seed rutile content height that is high, and preparing, is not suitable for the application requirement of denitration titanium dioxide high-specific surface area.
The object of the present invention is to provide it is a kind of it is easy to operate, at low cost, pollution-free, easily realize that industrialized additional hydrolyzing is brilliant
Kind preparation method, and the hydrolysis crystal seed activity prepared is high, the hole for the denitration titanium dioxide that crystal seed of the present invention is used to produce after hydrolyzing
Diameter can be controlled in 15~35nm, and pore passage structure is regular, pore-size distribution is narrow, and morphology microstructure is uniform-spherical, is suitable for de-
Extrusion, the forming process of denox catalyst production, crystal seed of the present invention improve the quality of domestic titanium dioxide, are conducive to be promoted domestic de-
The market competitiveness of nitre titanium dioxide.
Invention content
Place in view of the shortcomings of the prior art, the purpose of the present invention is to provide a kind of dioxide for denitration through use of titanium is additional
The preparation method of hydrolysis crystal seed, this method raw material are the black titanium liquid of Production By Sulfuric Acid Process, low for equipment requirements, the hydrolysis prepared
Activity of crystal seed is high, and the denitration titanium dioxide produced is suitable for the extrusion of denitrating catalyst production, forming process.
The purpose of the invention is achieved by the following technical solution:
A kind of preparation method of dioxide for denitration through use of titanium additional hydrolyzing seed crystal, which is characterized in that include the following steps:
Step1, the technical grade titanium liquid for meeting titanium liquid index is taken, is warming up to 70~90 DEG C,
Then Step2, the sodium hydroxide solution that compound concentration is 2.0~6.0mol/L are warming up to 70~90 DEG C;
Step3, the titanium liquid of Step1 is added in the sodium hydroxide solution obtained in Step2, after stirring evenly, is heated to
It 90~120 DEG C, then keeps the temperature 0~90min and is cured;
Step4, crystal seed stability reach 150ml hereinafter, reaction is hydrolyzed, and obtain crystal seed.
In order to preferably implement the present invention, the titanium liquid index in the Step1 is TiO2=170~220g/L, Ti3+=0.7
~2.7g/L, Fe2+/TiO2Value=1.55~2.00=0.25~0.35, F, proportion are 1.521~1.552.
It is specifically intended that the sodium hydroxide solution that cannot obtain Step2 in the Step3 is added to Step1 and obtains
Titanium liquid in, the crystal seed stability otherwise prepared is unstable.
Further, in the Step3, the adding proportion of sodium hydroxide solution and titanium liquid is molar ratio NaOH:TiO2=
0.35~7:1.
Preferably, the concentration of sodium hydroxide solution configured in the Step2 is 3.5~6.0mol/L.
Further, the concentration of sodium hydroxide solution configured in the Step2 is 3.5mol/L.
The present invention compared with the prior art, has the following advantages and advantageous effect:
1, the present invention using black titanium liquid as raw material, it is desirable that the concentration of sodium hydroxide and titanyl sulfate, by control sodium hydroxide with
The molar ratio of titanyl sulfate is prepared with the activity stabilized hydrolysis crystal seed of denitration titanium white production.
2, the aperture for the denitration titanium dioxide that crystal seed of the present invention is used to produce after hydrolyzing can be controlled in 15~30nm, pore passage structure
It is regular, pore-size distribution is narrow, morphology microstructure is uniform-spherical.
3, the present invention is to rely on the raw material of industry, and easy to operate, technological process is short, industrialized production easy to implement.
4, the present invention is low for equipment requirements, and the hydrolysis crystal seed activity prepared is high, and crystal seed of the present invention after hydrolyzing for producing
Denitration titanium dioxide be suitable for denitrating catalyst production extrusion, forming process.
Description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of the denitration titanium dioxide after crystal seed hydrolysis prepared by the embodiment of the present invention one.
Fig. 2 is the scanning electron microscope (SEM) photograph of the denitration titanium dioxide after crystal seed hydrolysis prepared by the embodiment of the present invention two.
Fig. 3 is the scanning electron microscope (SEM) photograph of the denitration titanium dioxide after crystal seed hydrolysis prepared by the embodiment of the present invention three.
Fig. 4 is the pore-size distribution of the denitration titanium dioxide after crystal seed hydrolysis prepared by the embodiment of the present invention one and embodiment two
Scheme, abscissa is aperture in figure, and ordinate is hole number.
Fig. 5 is the graph of pore diameter distribution of the denitration titanium dioxide after crystal seed hydrolysis prepared by the embodiment of the present invention three, horizontal in figure
Coordinate is aperture, and ordinate is hole number.
Specific implementation mode
The present invention is described in further detail with reference to embodiment, embodiments of the present invention are not limited thereto.
Embodiment one
Step1, it takes and meets titanium liquid index TiO2A concentration of 170g/L, Ti3+A concentration of 1.7g/L, Fe2+/TiO2Ratio be
0.35, the technical grade titanium liquid that F values are 1.73, proportion is 1.532, is warming up to 70 DEG C;
Step2, the sodium hydroxide solution that compound concentration is 2.3mol/L, are warming up to 70 DEG C;
Step3, titanium liquid is added in sodium hydroxide solution, after stirring evenly, temperature rises to 95 DEG C, heat preservation 15min curings;
Step4, crystal seed stability reach 120ml, and reaction is hydrolyzed, and obtain crystal seed;
In this example, by NaOH:TiO2=0.35:1(Molar ratio)Ratio prepare titanium liquid and sodium hydroxide solution.
Embodiment two
Step1, it takes and meets titanium liquid index TiO2A concentration of 170g/L, Ti3+A concentration of 0.9g/L, Fe2+/TiO2Ratio be
0.31, the technical grade titanium liquid that F values are 1.80, proportion is 1.525, is warming up to 75 DEG C;
Step2, the sodium hydroxide solution that compound concentration is 3.5mol/L, are warming up to 75 DEG C;
Step3, titanium liquid is added in sodium hydroxide solution, after stirring evenly, temperature rises to 100 DEG C, heat preservation 15min curings;
Step4, crystal seed stability reach 100ml, and reaction is hydrolyzed, and obtain crystal seed;
NaOH is pressed in this example:TiO2=1:1(Molar ratio)Ratio prepare titanium liquid and sodium hydroxide solution.
Embodiment three
Step1, it takes and meets titanium liquid index TiO2A concentration of 200g/L, Ti3+A concentration of 2.3g/L, Fe2+/TiO2Ratio be
0.29, the technical grade titanium liquid that F values are 1.90, proportion is 1.532, is warming up to 90 DEG C;
Step2, the sodium hydroxide solution that compound concentration is 6.0mol/L, are warming up to 90 DEG C;
Step3, titanium liquid is added in sodium hydroxide solution, after stirring evenly, temperature rises to 110 DEG C, heat preservation 8min curings;
Step4, crystal seed stability reach 90ml, and reaction is hydrolyzed, and obtain crystal seed;
NaOH is pressed in this example:TiO2=4.5:1(Molar ratio)Ratio prepare titanium liquid and sodium hydroxide solution.
In conclusion description through this embodiment, can make those skilled in the art preferably implement this programme.
Claims (6)
1. a kind of preparation method of dioxide for denitration through use of titanium additional hydrolyzing seed crystal, which is characterized in that include the following steps:
Step1, the technical grade titanium liquid for meeting titanium liquid index is taken, is warming up to 70~90 DEG C;
Then Step2, the sodium hydroxide solution that compound concentration is 2.0~6.0mol/L are warming up to 70~90 DEG C;
Step3, the titanium liquid of Step1 is added in the sodium hydroxide solution obtained in Step2, after stirring evenly, is heated to
It 90~120 DEG C, then keeps the temperature 0~90min and is cured;
Step4, crystal seed stability reach 150ml hereinafter, reaction is hydrolyzed, and obtain crystal seed.
2. a kind of preparation method of dioxide for denitration through use of titanium additional hydrolyzing seed crystal according to claim 1, it is characterised in that:
Titanium liquid index in the Step1 is TiO2=170~220g/L, Ti3+=0.7~2.7g/L, Fe2+/TiO2=0.25~0.35, F
Value=1.55~2.00, proportion are 1.521~1.552.
3. a kind of preparation method of dioxide for denitration through use of titanium additional hydrolyzing seed crystal according to claim 1, it is characterised in that:
The sodium hydroxide solution that cannot obtain Step2 in the Step3 is added in the titanium liquid that Step1 is obtained, the crystalline substance otherwise prepared
Kind stability is unstable.
4. a kind of preparation method of dioxide for denitration through use of titanium additional hydrolyzing seed crystal according to claim 1 or 3, feature exist
In:In the Step3, the adding proportion of sodium hydroxide solution and titanium liquid is molar ratio NaOH:TiO2=0.35~7:1.
5. a kind of preparation method of dioxide for denitration through use of titanium additional hydrolyzing seed crystal according to claim 1, it is characterised in that:
The concentration of sodium hydroxide solution configured in the Step2 is 3.5~6.0mol/L.
6. a kind of preparation method of dioxide for denitration through use of titanium additional hydrolyzing seed crystal, feature exist according to claim 1 or 5
In:The concentration of sodium hydroxide solution configured in the Step2 is 3.5mol/L.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114853057A (en) * | 2022-04-12 | 2022-08-05 | 安徽迪诺环保新材料科技有限公司 | Preparation method of titanium dioxide for denitration catalyst with high pore volume, small pore diameter and small specific surface area |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2012206058A (en) * | 2011-03-30 | 2012-10-25 | Nippon Shokubai Co Ltd | Denitration catalyst and denitrification method |
CN103288127A (en) * | 2013-05-13 | 2013-09-11 | 攀枝花市正源科技有限责任公司 | Catalyst titanium dioxide as well as a preparation method and a hydrolysis method thereof |
CN104150533A (en) * | 2014-08-08 | 2014-11-19 | 西南化工研究设计院有限公司 | Method for preparing anatase type titanium dioxide by acidolysis of clean titanium slag |
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2018
- 2018-06-08 CN CN201810589555.2A patent/CN108640150A/en active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2012206058A (en) * | 2011-03-30 | 2012-10-25 | Nippon Shokubai Co Ltd | Denitration catalyst and denitrification method |
CN103288127A (en) * | 2013-05-13 | 2013-09-11 | 攀枝花市正源科技有限责任公司 | Catalyst titanium dioxide as well as a preparation method and a hydrolysis method thereof |
CN104150533A (en) * | 2014-08-08 | 2014-11-19 | 西南化工研究设计院有限公司 | Method for preparing anatase type titanium dioxide by acidolysis of clean titanium slag |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114853057A (en) * | 2022-04-12 | 2022-08-05 | 安徽迪诺环保新材料科技有限公司 | Preparation method of titanium dioxide for denitration catalyst with high pore volume, small pore diameter and small specific surface area |
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Application publication date: 20181012 |