CN109321001A - A kind of serialization nano-TiO2The method of surface treatment - Google Patents
A kind of serialization nano-TiO2The method of surface treatment Download PDFInfo
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- CN109321001A CN109321001A CN201811048410.8A CN201811048410A CN109321001A CN 109321001 A CN109321001 A CN 109321001A CN 201811048410 A CN201811048410 A CN 201811048410A CN 109321001 A CN109321001 A CN 109321001A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/36—Compounds of titanium
- C09C1/3692—Combinations of treatments provided for in groups C09C1/3615 - C09C1/3684
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/36—Compounds of titanium
- C09C1/3607—Titanium dioxide
- C09C1/3615—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
- C09C1/363—Drying, calcination
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/36—Compounds of titanium
- C09C1/3607—Titanium dioxide
- C09C1/3653—Treatment with inorganic compounds
- C09C1/3661—Coating
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/36—Compounds of titanium
- C09C1/3607—Titanium dioxide
- C09C1/3669—Treatment with low-molecular organic compounds
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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- C09C1/3684—Treatment with organo-silicon compounds
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
The invention discloses a kind of continuous nano-TiOs2The method of surface treatment is obtained by techniques such as freeze-drying, silicon or aluminium cladding, organosilan or long chain fatty acids modifications.The present invention is by nano-TiO2Inorganic surface treatment and organic surface treatment organically combine, have the characteristics that process flow it is short, continuous operation and it is easy to operate, be easy to control, be suitable for industrialized production.The nano-TiO prepared simultaneously2Powder not only has good hydrophobicity, but also has excellent photostability, and further expand the application field of product.
Description
Technical field
The invention belongs to nano-functional material preparations and modified field, and in particular to a kind of serialization nano-TiO2At surface
The method of reason.
Background technique
Nano-titanium oxide (TiO2) it is a kind of novel inorganic ultraviolet shielding material, it is widely used in sunscreen cosmetic, applies
The fields such as material, plastics and chemical fibre.Since it has the characteristics that partial size is small, specific surface energy is high, easily occur to reunite to fill
The numerous characteristics of the nano material are waved in distribution；Meanwhile TiO2With stronger photochemical activity, under sunlight irradiation, easily
Cause the discoloration and degradation of organic matter in system；Furthermore its surface is in hydrophilic, fuel shedding quality, is suitably applied in polar system,
Such as aqueous solution, alcohol system.If being added into rubber, chemical fibre, plastics, ink, solvent based coating and oil-based cosmetic preparation etc. has
It is difficult evenly dispersed in machine application system, therefore nano-TiO cannot be fully demonstrated2Special efficacy.
In order to solve problem above, currently employed most method is surface-treated to it, and surface treatment is divided into nothing
Machine surface treatment and organic surface treatment.By inorganic coating, (general inorganic salts and ion itself using solubility are to nanometer
TiO2Flocculation, reuniting just has a certain impact) solve photolytic activity and agglomeration traits；It is solved by organically-modified organic
In phase the drawbacks of poor compatibility；It is few that they are organically combined into research and from the point of view of usually isolating them.Example
Such as: Chinese patent CN1454939A is by nano-TiO2Slurries at a certain temperature, maintain certain pH value, while sodium aluminate solution is added dropwise
Liquid and sulfuric acid solution in its surface-coated aluminum oxide, and are not directed to nano-TiO2Organic surface treatment.And Chinese patent
CN1982349A butyl titanate is to nano-TiO2Surface preparation is carried out, then carries out surface with methyl methacrylate
Polymerization, although improving nano-TiO2Dispersibility and stability in organic phase, but due to not carrying out at inorganic surfaces
Reason, leads to nano-TiO2Application field be extremely restricted.Therefore how nano-TiO is improved2The photostability of particle and having
Compatibility and dispersibility in machine phase are letter great research topics to be solved.
Summary of the invention
The technical problem to be solved in the present invention is that overcoming the shortcomings of in background technique, providing one kind can effectively inhibit to receive
Rice TiO2Photochemical activity can improve its compatibility and dispersibility in organic phase again；Nano-TiO is widened simultaneously2Using model
It encloses.The present invention passes through freeze-drying, silicon using the rutile titanium oxide of preparation described in 101698507 B of Chinese patent CN as raw material
Or the techniques such as aluminium coats, organosilan or long chain fatty acids are modified obtain.
The characterization step that the present invention uses are as follows:
1, nano-TiO2Preparation: with the progress of preparation method described in 101698507 B of Chinese patent CN；It obtains washing away foreign ion
Filter cake, be then freeze-dried, obtain rutile type nano TiO2Powder.
2, by nano-TiO in step 12The aqueous solution of powder alcohol is diluted to 10 ~ 30 wt% of solid content, heating water bath to 35
~ 75 DEG C, maintenance system pH is about 6 ~ 8, is stirred evenly.
3, silicon source or aluminium alcoholates are dissolved in the solution of the alcohol water ratio in step 2；And by a certain percentage be added step 2 mix it is molten
In liquid, stirs evenly and 1.5 ~ 5.5 h of insulation reaction, suction filtration, washing, dry, crushing can then obtain receiving by inorganic coating
Rice TiO2Powder.
4, after being kept the temperature in step 3, the alcohol solution of a certain proportion of organosiloxane or long chain fatty acids is added, stirs
Uniform and 0.5 ~ 3.5 h of insulation reaction is mixed, filters, wash, is dry, crushing can then be obtained by inorganic and organic surface treatment
Nano-TiO2Powder.
Wherein m(alcohol in step 2): m(water)=1:1 ~ 1:3；
Alcohols in step 2 is that ethyl alcohol, propylene glycol, butanediol, isopropanol etc. are one such；
Silicon source is that methyl orthosilicate, ethyl orthosilicate, positive silicic acid propyl ester etc. are one such in step 3；
Silicon source and nano-TiO in step 32Ratio are as follows: m(SiO2): m(TiO2)=1:20 ~ 1:5；Aluminium alcoholates and nano-TiO2Ratio
Example are as follows: m(Al2O3): m(TiO2)=1:25 ~ 3:20；
Aluminium alcoholates in step 3 is that aluminium ethylate, aluminium isopropoxide etc. are one such；
Organosilan in step 4 is dimethyl siloxane, dimethyl silicone polymer, octyltri-ethoxysilane, perfluoro capryl
Triethoxysilane etc. is one such；
Long chain fatty acids are that lauric acid, palmitinic acid, stearic acid etc. are one such in step 4；
Organosiloxane and nano-TiO in step 42Mass ratio are as follows: 1:50 ~ 1:10；
Long chain fatty acids and TiO in step 42Mass ratio are as follows: 1:20 ~ 3:20.
The present invention has the advantages that
The present invention provides a kind of serialization nano-TiO2Surface treatment method, not only available hydrophilic nano-TiO2And
Available hydrophobic nano-TiO2, the advantage is that:
1. nano-TiO2Surface treatment process avoids the use of solvable inorganic ion；Reduce nanometer in preparation process
TiO2Reunion generation.2. by nano-TiO2Inorganic surface treatment and organic surface treatment organically combine, have technique stream
Journey is short, continuous operation and easy to operate, the characteristics of being easy to control, and is suitable for industrialized production.3. reaction process by appropriate means,
Alcohol water can be recycled and is recycled, no discharge.4. the nano-TiO prepared2Powder not only has good hydrophobicity, but also
With excellent photostability.5. the nano-TiO of modification of the present invention2Have in fields such as cosmetics, rubber, plastics, coatings
Be widely applied.
Specific embodiment
Feature of present invention step is described in detail below, but protection scope of the present invention is not limited to the implementation
Example.
Embodiment 1
Nano-TiO of 1 kg by freeze-drying2The second alcohol and water of mass ratio 1:1 is added in powder, and totally 5 kg, is warming up to 55 DEG C,
Tune system pH is 8.Then 0.535 kg is added and contains 0.05kg SiO2Ethyl orthosilicate ethanol water, stir evenly,
5.5 h of insulation reaction at the temperature and pH.Filtering, washing, drying, crushing obtain the nano-TiO of inorganic silicon surface treatment2Powder
End.
Embodiment 2
Nano-TiO of 1 kg by freeze-drying2Second alcohol and water totally 5 kg of mass ratio 1:1 is added in powder, is warming up to 55 DEG C,
Tune system pH is 8.Then 0.535 kg is added and contains 0.05kg SiO2Ethyl orthosilicate ethanol water, stir evenly,
5.5 h of insulation reaction under the temperature and pH.Then 1.2 kg are added and contain 0.06kg dimethyl silicone polymer ethanol water, stir
It mixes uniformly, 0.5 h of insulation reaction at the temperature and pH.After reaction, be filtered, washed, dry, crush obtain it is inorganic modified
With the nano-TiO of organic surface treatment2Powder.
Embodiment 3
Nano-TiO of 1 kg by freeze-drying2Isopropyl alcohol and water totally 10 kg of mass ratio 1:2 is added in powder, is warming up to 75
DEG C, adjusting system pH is 6.Then 1.07 kg are added and contain 0.1kg SiO2Positive silicic acid propyl ester isopropanol water solution, stirring is equal
It is even, 1.5 h of insulation reaction at the temperature and pH.Then 0.4 kg is added and contains 0.02kg octyltri-ethoxysilane isopropanol
Aqueous solution stirs evenly, 2 h of insulation reaction at the temperature and pH.After reaction, it is filtered, washed, dries, crushing and obtain
The nano-TiO of inorganic modified and organic surface treatment2Powder.
Embodiment 4
Nano-TiO of 1 kg by freeze-drying2The propylene glycol and water totally 3.33 kg of mass ratio 1:3 is added in powder, is warming up to 35
DEG C, adjusting system pH is 7.Then 2.14 kg are added and contain 0.15kg SiO2Methyl orthosilicate aqueous solution of propylene glycol, stirring is equal
It is even, 3.5 h of insulation reaction at the temperature and pH.Then the dimethyl siloxane propylene glycol water that 2.0 kg contain 0.1kg is added
Solution stirs evenly, 3.5 h of insulation reaction at the temperature and pH.After reaction, it is filtered, washed, dries, crushing and obtain
The nano-TiO of inorganic modified and organic surface treatment2Powder.
Embodiment 5
Nano-TiO of 1 kg by freeze-drying2The butanediol and water totally 5 kg of mass ratio 1:2 is added in powder, is warming up to 55
DEG C, adjusting system pH is 6.Then 2.14 kg are added and contain 0.15kg SiO2Ethyl orthosilicate butanediol aqueous solution, stirring is equal
It is even, 1.5 h of insulation reaction at the temperature and pH.Then 0.4 kg is added and contains 0.02kg perfluoro capryl triethoxysilane fourth
Two alcohol solutions, stir evenly, 2 h of insulation reaction at the temperature and pH.After reaction, it is filtered, washed, dries, crushes
Obtain the nano-TiO of inorganic modified and organic surface treatment2Powder.
Embodiment 6
Nano-TiO of 1 kg by freeze-drying2Second alcohol and water totally 5 kg of mass ratio 1:1 is added in powder, is warming up to 55 DEG C,
Tune system pH is 8.Then 1.60 kg are added and contain 0.04kg Al2O3Aluminium isopropoxide ethanol water, stir evenly, at this
5.5 h of insulation reaction under temperature and pH.Filtering, washing, drying, crushing obtain the nano-TiO of inorganic aluminum surface treatment2Powder.
Embodiment 7
Nano-TiO of 1 kg by freeze-drying2Second alcohol and water totally 5 kg of mass ratio 1:1 is added in powder, is warming up to 55 DEG C,
Tune system pH is 8.Then 1.60 kg are added and contain 0.04kg Al2O3Aluminium isopropoxide ethanol water, stir evenly, at this
5.5 h of insulation reaction under temperature and pH.Then 1.0 kg are added and contain 0.05kg stearic acid ethanol water, stir evenly,
0.5 h of insulation reaction under the temperature and pH.After reaction, it is filtered, washed, dries, crushing and obtain inorganic modified and organic table
The nano-TiO of surface treatment2Powder.
Embodiment 8
Nano-TiO of 1 kg by freeze-drying2Isopropyl alcohol and water totally 10 kg of mass ratio 1:2 is added in powder, is warming up to 75
DEG C, adjusting system pH is 6.Then 1.9 kg are added and contain 0.1kg Al2O3Aluminium ethylate isopropanol water solution, stir evenly, at this
1.5 h of insulation reaction under temperature and pH.Then 3.0 kg are added and contain 0.15kg lauric acid isopropanol water solution, stir evenly,
2 h of insulation reaction at the temperature and pH.After reaction, it is filtered, washed, dries, crushing and obtain inorganic modified and organic table
The nano-TiO of surface treatment2Powder.
Embodiment 9
Nano-TiO of 1 kg by freeze-drying2The propylene glycol and water totally 3.33 kg of mass ratio 1:3 is added in powder, is warming up to 35
DEG C, adjusting system pH is 7.Then 2.14 kg are added and contain 0.15kg Al2O3Aluminium ethylate aqueous solution of propylene glycol, stir evenly,
3.5 h of insulation reaction under the temperature and pH.Then 2.0 kg are added and contain 0.1kg palmitinic acid aqueous solution of propylene glycol, stir evenly,
3.5 h of insulation reaction at the temperature and pH.After reaction, be filtered, washed, dry, crush obtain it is inorganic modified and organic
The nano-TiO of surface treatment2Powder.
Embodiment 10
Nano-TiO of 1 kg by freeze-drying2The butanediol and water totally 5 kg of mass ratio 1:2 is added in powder, is warming up to 55
DEG C, adjusting system pH is 6.Then 1.6 kg are added and contain 0.04kg Al2O3Aluminium isopropoxide butanediol aqueous solution, stir evenly,
1.5 h of insulation reaction at the temperature and pH.Then 2.0 kg are added and contain 0.1kg stearic acid butanediol aqueous solution, stirring is equal
It is even, 2 h of insulation reaction at the temperature and pH.After reaction, be filtered, washed, dry, crush obtain it is inorganic modified and organic
The nano-TiO of surface treatment2Powder.
Comparative example 1
It is proceeded through with preparation method described in 101698507 B of Chinese patent CN and is filtered, washed, dries, crushing and obtain rutile
Type nano-TiO2Powder.
Comparative example 2
Nano-TiO of 1 kg by freeze-drying2Second alcohol and water totally 5 kg of mass ratio 1:1 is added in powder, is warming up to 55 DEG C,
Tune system pH is 8.Then 0.535 kg is added and contains 0.05kg SiO2Ethyl orthosilicate ethanol water, stir evenly,
5.5 h of insulation reaction under the temperature and pH.Then 1.0 kg are added and contain 0.05kg stearic acid ethanol water, stir evenly,
0.5 h of insulation reaction at the temperature and pH.After reaction, be filtered, washed, dry, crush obtain it is inorganic modified and organic
The nano-TiO of surface treatment2Powder.
Comparative example 3
Nano-TiO of 1 kg by freeze-drying2Second alcohol and water totally 5 kg of mass ratio 1:1 is added in powder, is warming up to 55 DEG C,
Tune system pH is 8.Then 1.60 kg are added and contain 0.04kg Al2O3Aluminium isopropoxide ethanol water, stir evenly, at this
5.5 h of insulation reaction under temperature and pH.Then 1.2 kg are added and contain 0.06kg dimethyl silicone polymer ethanol water, stir
Uniformly, 0.5 h of insulation reaction at the temperature and pH.After reaction, be filtered, washed, dry, crush obtain it is inorganic modified and
The nano-TiO of organic surface treatment2Powder.
Nano-TiO2The evaluation of photostability stability
By the nano-TiO after surface treatment2With 1-3 butanediol be in mass ratio 1:1 ratio be uniformly mixed, ground in mortar
Mill takes out mixture and is applied on a glass slide by certain thickness when being ground to certain, with another glass slide and applies
The glass slide covered slowly forces together, sample panel is placed on irradiate 1 h under high-pressure sodium lamp (250 W) after take out, with SC-80C entirely from
Dynamic colour difference meter test light shines L, a, b and L*, a*, b* of the sample of front and back, and the color of sample before and after illumination is calculated with following formula
Then difference takes the average value of color difference (△ E) to obtain the final color difference before and after sample illumination.The calculation formula of color difference is as follows:
△E=[(L-L*)2+(a-a*)2+(b-b*)2]1/2
△ E is color difference size, and L indicates bright dark ,+indicate partially bright ,-indicate partially dark；A indicates red green ,+indicate partially red ,-indicate inclined
It is green；B indicates champac ,+indicate partially yellow ,-indicate partially blue.When △ E is bigger, illustrate nano-TiO2Photochemical activity it is higher, more
It is low, illustrate TiO2Light resistance it is better.
Nano-TiO2Hydrophobic performance evaluation
Weigh nano-TiO after 3 g are surface-treated in the balance2Sample tablet press machine in flakes, then exists under 10 Mpa pressure
The water contact angle of test sample under DSA25 type optical contact angle measuring instrument, each sample are surveyed three times, take its average value as sample
Water contact angle numerical value.Water contact angle is bigger, indicates nano-TiO2Hydrophobicity is better.
The performance table of 1 sample of table
| Color difference △ E | Water contact angle/° | |
| Embodiment 1 | 5.4 | 32.0 |
| Embodiment 2 | 3.7 | 131.3 |
| Embodiment 3 | 4.2 | 148.9 |
| Embodiment 4 | 4.7 | 133.2 |
| Embodiment 5 | 3.9 | 151.6 |
| Embodiment 6 | 6.1 | 29.8 |
| Embodiment 7 | 4.9 | 129.7 |
| Embodiment 8 | 4.7 | 137.4 |
| Embodiment 9 | 4.4 | 139.2 |
| Embodiment 10 | 4.0 | 138.3 |
| Comparative example 1 | 39.8 | 27.9 |
| Comparative example 2 | 4.6 | 95.0 |
| Comparative example 3 | 4.3 | 91.5 |
As shown in Table 1, the nano-TiO that the present invention prepares2Powder not only has good hydrophobicity, but also has excellent light
Stability, and hydrophobicity powder that must be prepared under specific process conditions has preferable hydrophobic performance, preparation process
It cannot be adjusted and exchange.
Claims (4)
1. a kind of serialization nano-TiO2The method of surface treatment, it is characterised in that: the serialization nano-TiO2The side of surface treatment
Method is as follows:
Nano-TiO2Preparation: with the progress of preparation method described in 101698507 B of Chinese patent CN；Obtain washing away the filter of foreign ion
Then cake is freeze-dried, rutile type nano TiO is obtained2Powder；
By nano-TiO in (1)2The aqueous solution of powder alcohol is diluted to 10 ~ 30 wt% of solid content, and heating water bath is to 35 ~ 75 DEG C, dimension
The system pH of holding is about 6 ~ 8, is stirred evenly；
It with the aqueous dissolution silicon source or aluminium alcoholates of alcohol, is added in (2) mixed solution, stirs evenly simultaneously 1.5 ~ 5.5 h of insulation reaction,
It filters, washing, drying, crush the nano-TiO that can then obtain by inorganic coating2Powder；
After to heat preservation in (3), the alcohol solution of organosiloxane or long chain fatty acids is added, stirs evenly simultaneously insulation reaction
0.5 ~ 3.5 h is filtered, washing, drying, is crushed the nano-TiO that can then obtain by inorganic and organic surface treatment2Powder.
2. a kind of serialization nano-TiO told such as claim 12The method of surface treatment, it is characterised in that: told step
(2), in (3) alcohol water quality ratio be m(alcohol): m(water)=1:1 ~ 1:3, and alcohols be ethyl alcohol, propylene glycol, butanediol, isopropanol its
One of.
3. a kind of serialization nano-TiO told such as claim 12The method of surface treatment, it is characterised in that: told step (3)
Middle silicon source is that methyl orthosilicate, ethyl orthosilicate, positive silicic acid propyl ester are one such,
And silicon source and nano-TiO2Mass ratio are as follows: m(SiO2): m(TiO2)=1:20 ~ 1:5；
Aluminium alcoholates in told step (3) is one such for aluminium ethylate, aluminium isopropoxide etc., and aluminium alcoholates and nano-TiO2Mass ratio
Are as follows: m(Al2O3): m(TiO2)=1:25 ~ 3:20.
4. a kind of serialization nano-TiO told such as claim 12The method of surface treatment, it is characterised in that: told step (4)
In organosilan be dimethyl siloxane, dimethyl silicone polymer, octyltri-ethoxysilane, perfluoro capryl triethoxysilicane
Alkane etc. is one such, and organosiloxane and nano-TiO2Mass ratio are as follows: 1:50 ~ 1:10；Long-chain rouge in the step (4)
Fat acid is that lauric acid, palmitinic acid, stearic acid are one such, and long-chain fat and TiO2Mass ratio are as follows: 1:20 ~ 3:20.
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| CN201811048410.8A CN109321001A (en) | 2018-09-10 | 2018-09-10 | A kind of serialization nano-TiO2The method of surface treatment |
| PCT/CN2018/116404 WO2020052070A1 (en) | 2018-09-10 | 2018-11-20 | Continuous nanometer tio2 surface treatment method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110669564A (en) * | 2019-08-31 | 2020-01-10 | 佛山市南海区里水镇经济促进局 | Oleophylic nano titanium dioxide and preparation method and application thereof |
| CN111484755A (en) * | 2020-04-09 | 2020-08-04 | 行謇人工智能科技(上海)有限责任公司 | Lauric acid modified nano titanium dioxide and preparation method and application thereof |
| CN112645382A (en) * | 2019-10-09 | 2021-04-13 | 万华化学集团股份有限公司 | Preparation method of nano titanium dioxide, nano titanium dioxide and application |
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| DE102004030093A1 (en) * | 2004-06-22 | 2006-01-12 | Degussa Ag | Metal oxide sol, layer and moldings produced therewith |
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| CN105860648B (en) * | 2016-05-05 | 2018-09-14 | 焦作市裕盛钛业有限公司 | A kind of special cladding titanium dioxide of ink and preparation method thereof |
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2018
- 2018-09-10 CN CN201811048410.8A patent/CN109321001A/en active Pending
- 2018-11-20 WO PCT/CN2018/116404 patent/WO2020052070A1/en active Application Filing
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| CN101698507B (en) * | 2009-11-23 | 2011-11-23 | 江苏河海纳米科技股份有限公司 | Method for quickly preparing rutile phase nano titanium dioxide |
| CN102199367A (en) * | 2011-03-30 | 2011-09-28 | 中国科学院宁波材料技术与工程研究所 | Method for preparing titanium dioxide pigment with high-temperature resistance |
| CN102924979A (en) * | 2012-11-05 | 2013-02-13 | 昆明理工大学 | Method for preparing inorganic and organic coating titanium dioxide |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110669564A (en) * | 2019-08-31 | 2020-01-10 | 佛山市南海区里水镇经济促进局 | Oleophylic nano titanium dioxide and preparation method and application thereof |
| CN112645382A (en) * | 2019-10-09 | 2021-04-13 | 万华化学集团股份有限公司 | Preparation method of nano titanium dioxide, nano titanium dioxide and application |
| CN111484755A (en) * | 2020-04-09 | 2020-08-04 | 行謇人工智能科技(上海)有限责任公司 | Lauric acid modified nano titanium dioxide and preparation method and application thereof |
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