CN107324381A - A kind of preparation method of nano-titanium dioxide powder - Google Patents
A kind of preparation method of nano-titanium dioxide powder Download PDFInfo
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- CN107324381A CN107324381A CN201710572785.3A CN201710572785A CN107324381A CN 107324381 A CN107324381 A CN 107324381A CN 201710572785 A CN201710572785 A CN 201710572785A CN 107324381 A CN107324381 A CN 107324381A
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- 239000000843 powder Substances 0.000 title claims abstract description 46
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000007788 liquid Substances 0.000 claims abstract description 17
- KWYHDKDOAIKMQN-UHFFFAOYSA-N N,N,N',N'-tetramethylethylenediamine Chemical compound CN(C)CCN(C)C KWYHDKDOAIKMQN-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 16
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000001393 triammonium citrate Substances 0.000 claims abstract description 16
- 235000011046 triammonium citrate Nutrition 0.000 claims abstract description 16
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 7
- 239000007864 aqueous solution Substances 0.000 claims description 28
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 26
- 239000010936 titanium Substances 0.000 claims description 26
- 229910052719 titanium Inorganic materials 0.000 claims description 26
- 239000000243 solution Substances 0.000 claims description 25
- CCJAYIGMMRQRAO-UHFFFAOYSA-N 2-[4-[(2-hydroxyphenyl)methylideneamino]butyliminomethyl]phenol Chemical compound OC1=CC=CC=C1C=NCCCCN=CC1=CC=CC=C1O CCJAYIGMMRQRAO-UHFFFAOYSA-N 0.000 claims description 21
- 238000013019 agitation Methods 0.000 claims description 15
- 239000011837 N,N-methylenebisacrylamide Substances 0.000 claims description 7
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 claims description 7
- 238000003801 milling Methods 0.000 claims description 5
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N methanol Natural products OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O ammonium group Chemical group [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims 2
- 150000001412 amines Chemical class 0.000 claims 1
- KFIGICHILYTCJF-UHFFFAOYSA-N n'-methylethane-1,2-diamine Chemical compound CNCCN KFIGICHILYTCJF-UHFFFAOYSA-N 0.000 claims 1
- 150000004968 peroxymonosulfuric acids Chemical class 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 22
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 19
- 150000004703 alkoxides Chemical class 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 3
- 239000002184 metal Substances 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 150000003839 salts Chemical class 0.000 abstract description 3
- 238000001354 calcination Methods 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 abstract description 2
- 239000003431 cross linking reagent Substances 0.000 abstract description 2
- 239000004615 ingredient Substances 0.000 abstract description 2
- 239000003999 initiator Substances 0.000 abstract description 2
- 150000002500 ions Chemical class 0.000 abstract description 2
- 239000000178 monomer Substances 0.000 abstract description 2
- 239000011858 nanopowder Substances 0.000 abstract description 2
- 239000002243 precursor Substances 0.000 abstract description 2
- FIKFOOMAUXPBJM-UHFFFAOYSA-N hepta-2,5-dienediamide Chemical class NC(=O)C=CCC=CC(N)=O FIKFOOMAUXPBJM-UHFFFAOYSA-N 0.000 abstract 1
- 239000004408 titanium dioxide Substances 0.000 description 6
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 6
- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 239000008187 granular material Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000002781 deodorant agent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000000713 high-energy ball milling Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000004153 renaturation Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000012808 vapor phase Substances 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Catalysts (AREA)
Abstract
The present invention relates to a kind of preparation method of nano-titanium dioxide powder, belong to nano-powder preparing technical field.The present invention prepares nano-titanium dioxide powder using polymer-network gel method, using butyl titanate, Triammonium citrate as raw material, is configured to precursor liquid；Using N NMAs monomer, N N methylene-bisacrylamides are crosslinking agent, and ammonium persulfate is initiator, and tetramethylethylenediamine is catalyst, and with ammoniacal liquor mode control ph is added dropwise, formation contains TiO2Polyacrylamide-gel, by gel drying, by controlling calcining heat to obtain nano-TiO2Powder.The inventive method is simple to ingredient requirement, and water-soluble inorganic salts are only needed during Doped ions, it is to avoid use expensive metal alkoxide；With technique is simple, aggregate velocity is fast, it is applied widely the features such as；The nano-titanium dioxide powder purity that the inventive method is prepared is high, and powder dispersity is good.
Description
Technical field
The present invention relates to a kind of preparation method of nano-titanium dioxide powder, belong to nano-powder preparing technical field.
Background technology
In traditional industries, titanium dioxide is widely used in the fields such as pigment, coating, plastics, papermaking, or even because its is nontoxic
Innocuousness and be added into edible cosmetic product, with going deep into for research, many other advantageous property of titanium dioxide is found, especially
It is the peculiar property as semi-conducting material based on it, brought for us generated electricity using sunshine, degradation of contaminant,
New trial in terms of hydrogen production by water decomposition.Nano titanium oxide is the material of a high comprehensive performance, by various modified
It is more prominent for certain aspect effect.In addition to traditional ripe application, new function titanium dioxide is displayed that in all many-sides
In terms of its existent value, such as dye-sensitized cell, environment-friendly deodorant, new coating, Medical sterilization, light decomposition water.Titanium dioxide
The method of titanium synthesis has a lot, divides to get up to have vapor phase method, liquid phase method, solid phase method, no matter such as what is had is divided into Physical, chemical method,
What, the preparation technology of titanium dioxide is quite ripe.But generally speaking, different preparation methods have to Titanium Dioxide performance
Very big influence, therefore, the preparation method of nano titanium oxide is particularly important.There is gas phase fire with regard to the doping means of present comparative maturity
Flame, high-energy ball milling, induced with laser, hydro-thermal method, the precipitation method, magnetron sputtering, gel method etc..But these method generally existings
The high, shortcoming that aggregate velocity is slow and cost is high is required to process conditions.
The content of the invention
In view of the deficiencies of the prior art, the present invention provides one kind uses polymer-network gel method to prepare nano titanium oxide
The method of powder, i.e., prepare nano-titanium dioxide powder, with butyl titanate, Triammonium citrate using polymer-network gel method
For raw material, precursor liquid is configured to；Using N hydroxymethyl acrylamide as monomer, N-N- methylene-bisacrylamides are crosslinking agent,
Ammonium persulfate is initiator, and tetramethylethylenediamine is catalyst, and with ammoniacal liquor mode control ph is added dropwise, formation contains TiO2Height
Molecular network gel, by gel drying, by controlling calcining heat to obtain nano-TiO2Powder.The inventive method has to raw material
It is required that it is simple, water-soluble inorganic salts are only needed during Doped ions, it is to avoid using expensive metal alkoxide, technique is simple,
Aggregate velocity is fast, the features such as applied widely, and nano-titanium dioxide powder purity height, the powder dispersity of preparation are good.
A kind of preparation method of nano-titanium dioxide powder, it is characterised in that concretely comprise the following steps：
（1）Under agitation, butyl titanate is dissolved in the Triammonium citrate aqueous solution and be well mixed, stood, remove layer
Clear liquid produces titanium clarified solution A；
（2）Under agitation, it is 8.0 ~ 10.0 to adjust titanium clarified solution A pH value with ammoniacal liquor, then by N- methylol acryloyls
Amine and N,N methylene bis acrylamide are dissolved in titanium clarified solution A and obtain mixed liquid B；
（3）Under agitation, ammonium persulfate aqueous solution and the tetramethylethylenediamine aqueous solution are added to step（2）Gained is mixed
1 ~ 15min is reacted in liquid B and produces polyacrylamide-gel；
（4）By step（3）The drying of gained polyacrylamide-gel, milling, roasting produce nano-titanium dioxide powder；
The step（1）The concentration of the middle Triammonium citrate aqueous solution is 1.0 ~ 1.2mol/L, in titanium clarified solution A butyl titanate with
The mol ratio of Triammonium citrate is 1:(1~1.2 )；
The step（2）Middle N hydroxymethyl acrylamide and titanium clarified solution A volume ratio are (3 ~ 7):100, N, N- di-2-ethylhexylphosphine oxide
The mass ratio of acrylamide and N hydroxymethyl acrylamide is 1:(3~8)；
The step（3）The mass percent concentration of middle ammonium persulfate aqueous solution is 30 ~ 50 %, ammonium persulfate and N- methylols third
The mass ratio of acrylamide is 6 ~ 8%；The mass percent concentration of the tetramethylethylenediamine aqueous solution is 30 ~ 50 %, tetramethylethylenediamine
Mass ratio with N hydroxymethyl acrylamide is 6 ~ 8%；
The step（4）The temperature of middle roasting is 500 ~ 800 DEG C, and roasting time is 3 ~ 7h.
Beneficial effects of the present invention：
（1）The method that the present invention prepares nano-titanium dioxide powder using polymer-network gel method is simple to ingredient requirement, mixes
Water-soluble inorganic salts during heteroion, it is to avoid use expensive metal alkoxide；
（2）The method that the present invention prepares nano-titanium dioxide powder using polymer-network gel method has technique simple, can weigh
Renaturation is good, aggregate velocity is fast, it is applied widely the features such as；
（3）The product purity of nano-titanium dioxide powder prepared by the present invention is high, powder uniformity is good.
Brief description of the drawings
Fig. 1 schemes for the nano-titanium dioxide powder SEM of embodiment 1；
Fig. 2 schemes for the nano-titanium dioxide powder SEM of embodiment 2；
Fig. 3 schemes for the nano-titanium dioxide powder SEM of embodiment 3.
Embodiment
The present invention is described in further detail with reference to embodiment, but protection scope of the present invention is not limited
In the content.
Embodiment 1：A kind of preparation method of nano-titanium dioxide powder, is concretely comprised the following steps：
（1）Under agitation, butyl titanate is dissolved in the Triammonium citrate aqueous solution and be well mixed, stood, remove layer
Clear liquid produces titanium clarified solution A；Wherein the concentration of the Triammonium citrate aqueous solution is 1mol/L, in titanium clarified solution A butyl titanate with
The mol ratio of Triammonium citrate is 1:1；
（2）Under agitation, it is 8.0 to adjust titanium clarified solution A pH value with ammoniacal liquor, then by N hydroxymethyl acrylamide and N,
N- methylene-bisacrylamides are dissolved in titanium clarified solution A and obtain mixed liquid B；Wherein N hydroxymethyl acrylamide and titanium clarified solution A
Volume ratio be 3:The mass ratio of 100, N, N- methylene-bisacrylamide and N hydroxymethyl acrylamide is 1:3.
（3）Under agitation, ammonium persulfate aqueous solution and the tetramethylethylenediamine aqueous solution are added to step（2）Gained
1min is reacted in mixed liquid B and produces polyacrylamide-gel；Wherein the mass percent concentration of ammonium persulfate aqueous solution is 30%,
The mass ratio of ammonium persulfate and N hydroxymethyl acrylamide is 6:100, the mass percent concentration of the tetramethylethylenediamine aqueous solution
For 30%, the mass ratio of tetramethylethylenediamine and N hydroxymethyl acrylamide is 6:100；
（4）By step（3）The drying of gained polyacrylamide-gel, milling, roasting produce nano-titanium dioxide powder, wherein being calcined
Temperature be 500 DEG C, roasting time is 3h；
The SEM figures of nano-titanium dioxide powder manufactured in the present embodiment are as shown in Figure 1.From fig. 1, it can be seen that powder granule is in spherical,
Agglomeration is few between particle, good dispersion.This illustrates TiO manufactured in the present embodiment2Degree of grain refinement is high, and uniformity is good, increases
The big specific surface area of powder, is conducive to improving nano-titanium dioxide powder photocatalytic activity.
Embodiment 2：A kind of preparation method of nano-titanium dioxide powder, is concretely comprised the following steps：
（1）Under agitation, butyl titanate is dissolved in the Triammonium citrate aqueous solution and be well mixed, stood, remove layer
Clear liquid produces titanium clarified solution A；Wherein the concentration of the Triammonium citrate aqueous solution is butyl titanate in 1.1mol/L, titanium clarified solution A
Mol ratio with Triammonium citrate is 1: 1.1；
（2）Under agitation, it is 9.0 to adjust titanium clarified solution A pH value with ammoniacal liquor, then by N hydroxymethyl acrylamide and N,
N- methylene-bisacrylamides are dissolved in titanium clarified solution A and obtain mixed liquid B；Wherein N hydroxymethyl acrylamide and titanium clarified solution A
Volume ratio be 5:The mass ratio of 100, N, N- methylene-bisacrylamide and N hydroxymethyl acrylamide is 1:6.
（3）Under agitation, ammonium persulfate aqueous solution and the tetramethylethylenediamine aqueous solution are added to step（2）Gained
8min is reacted in mixed liquid B and produces polyacrylamide-gel；Wherein the mass percent concentration of ammonium persulfate aqueous solution is 40%,
The mass ratio of ammonium persulfate and N hydroxymethyl acrylamide is 7:100, the mass percent concentration of the tetramethylethylenediamine aqueous solution
40%, the mass ratio of tetramethylethylenediamine and N hydroxymethyl acrylamide is 7:100；
（4）By step（3）The drying of gained polyacrylamide-gel, milling, roasting produce nano-titanium dioxide powder, wherein being calcined
Temperature be 650 DEG C, roasting time is 5h；
The SEM figures of nano-titanium dioxide powder manufactured in the present embodiment are as shown in Figure 2.As can be seen from Figure 2, powder granule is in spherical,
Agglomeration is few between particle, good dispersion.This illustrates TiO manufactured in the present embodiment2Degree of grain refinement is high, and uniformity is good, increases
The big specific surface area of powder, is conducive to improving nano-titanium dioxide powder photocatalytic activity.
Embodiment 3：A kind of preparation method of nano-titanium dioxide powder, is concretely comprised the following steps：
（1）Under agitation, butyl titanate is dissolved in the Triammonium citrate aqueous solution and be well mixed, stood, remove layer
Clear liquid produces titanium clarified solution A；Wherein the concentration of the Triammonium citrate aqueous solution is butyl titanate in 1.2mol/L, titanium clarified solution A
Mol ratio with Triammonium citrate is 1: 1.2；
（2）Under agitation, the pH value for adjusting titanium clarified solution A with ammoniacal liquor is 10.0, then by N hydroxymethyl acrylamide and
N,N methylene bis acrylamide is dissolved in titanium clarified solution A and obtains mixed liquid B；Wherein N hydroxymethyl acrylamide and titanium clarified solution
A volume ratio is 7:The mass ratio of 100, N, N- methylene-bisacrylamide and N hydroxymethyl acrylamide is 1:8.
（3）Under agitation, ammonium persulfate aqueous solution and the tetramethylethylenediamine aqueous solution are added to step（2）Gained
15min is reacted in mixed liquid B and produces polyacrylamide-gel；Wherein the mass percent concentration of ammonium persulfate aqueous solution is 50%,
The mass ratio of ammonium persulfate and N hydroxymethyl acrylamide is 8:100, the mass percent concentration of the tetramethylethylenediamine aqueous solution
For 50%, the mass ratio of tetramethylethylenediamine and N hydroxymethyl acrylamide is 8:100；
（4）By step（3）The drying of gained polyacrylamide-gel, milling, roasting produce nano-titanium dioxide powder, wherein being calcined
Temperature be 800 DEG C, roasting time is 7h；
The SEM figures of nano-titanium dioxide powder manufactured in the present embodiment are as shown in Figure 3.As can be seen from Figure 3, powder granule is in spherical,
Agglomeration is few between particle, good dispersion.This illustrates TiO manufactured in the present embodiment2Degree of grain refinement is high, and uniformity is good, increases
The big specific surface area of powder, is conducive to improving nano-titanium dioxide powder photocatalytic activity.
Claims (5)
1. a kind of preparation method of nano-titanium dioxide powder, it is characterised in that concretely comprise the following steps：
（1）Under agitation, butyl titanate is dissolved in the Triammonium citrate aqueous solution and be well mixed, stood, remove layer
Clear liquid produces titanium clarified solution A；
（2）Under agitation, it is 8.0 ~ 10.0 to adjust titanium clarified solution A pH value with ammoniacal liquor, then by N- methylol acryloyls
Amine and N,N methylene bis acrylamide are dissolved in titanium clarified solution A and obtain mixed liquid B；
（3）Under agitation, ammonium persulfate aqueous solution and the tetramethylethylenediamine aqueous solution are added to step（2）Gained is mixed
1 ~ 15min is reacted in liquid B and produces polyacrylamide-gel；
（4）By step（3）The drying of gained polyacrylamide-gel, milling, roasting produce nano-titanium dioxide powder.
2. the preparation method of nano-titanium dioxide powder according to claim 1, it is characterised in that：Step（1）Middle citric acid
The concentration of three aqueous ammoniums is that the mol ratio of butyl titanate and Triammonium citrate in 1.0 ~ 1.2mol/L, titanium clarified solution A is 1:
(1~1.2 )。
3. the preparation method of nano-titanium dioxide powder according to claim 1, it is characterised in that：Step（2）Middle N- hydroxyls first
Base acrylamide and titanium clarified solution A volume ratio are (3 ~ 7):100, N, N- methylene-bisacrylamide and N- methylol acryloyls
The mass ratio of amine is 1:(3~8).
4. the preparation method of nano-titanium dioxide powder according to claim 1, it is characterised in that：Step（3）Middle persulfuric acid
The mass percent concentration of aqueous ammonium is 30 ~ 50 %, and the mass ratio of ammonium persulfate and N hydroxymethyl acrylamide is 6 ~ 8%；Four
The mass percent concentration of the methyl ethylenediamine aqueous solution is 30 ~ 50 %, tetramethylethylenediamine and N hydroxymethyl acrylamide matter
Amount is than being 6 ~ 8%.
5. the preparation method of nano-titanium dioxide powder according to claim 1, it is characterised in that：Step（4）Middle roasting
Temperature is 500 ~ 800 DEG C, and roasting time is 3 ~ 7h.
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| CN112850733A (en) * | 2021-03-01 | 2021-05-28 | 江苏省宜兴电子器件总厂有限公司 | HTCC packaging tube shell glass pigment, preparation method and application |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109205667A (en) * | 2018-11-08 | 2019-01-15 | 绍兴文理学院 | A kind of preparation method of nano-titanium dioxide |
| CN110694580A (en) * | 2019-10-14 | 2020-01-17 | 盐城师范学院 | Preparation method of titanium dioxide porous pellets |
| CN112850733A (en) * | 2021-03-01 | 2021-05-28 | 江苏省宜兴电子器件总厂有限公司 | HTCC packaging tube shell glass pigment, preparation method and application |
| CN112850733B (en) * | 2021-03-01 | 2023-06-09 | 江苏省宜兴电子器件总厂有限公司 | HTCC packaging tube shell glass pigment, preparation method and application |
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