CN106590060A - Method of allowing nano titanium dioxide to be evenly distributed in polymer - Google Patents
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- CN106590060A CN106590060A CN201611041467.6A CN201611041467A CN106590060A CN 106590060 A CN106590060 A CN 106590060A CN 201611041467 A CN201611041467 A CN 201611041467A CN 106590060 A CN106590060 A CN 106590060A
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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
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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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
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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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
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
- C09C3/063—Coating
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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
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/10—Treatment with macromolecular organic compounds
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Abstract
The invention relates to the field of nano materials, and particularly discloses a method of allowing nano titanium dioxide to be evenly distributed in a polymer. The method comprises the following steps: (1) nano silver is prepared; (2) nano titanium dioxide is prepared; (3) nano silver is loaded to the surface of nano titanium dioxide, and a nano titanium dioxide silver-loaded composite material is obtained; (4) a film-forming agent, a defoaming agent and a flatting agent are added to the nano titanium dioxide silver-loaded composite material; and (5) a mixture obtained in the step (4) is uniformly mixed in the polymer. Nano titanium dioxide prepared by the method can be evenly dispersed and composited in the polymer in a nano scale, and has good dispersing performance, and the possibilities of aggregation and sediment phenomena are low.
Description
Technical field
The present invention relates to field of nanometer material technology, specifically, being related to one kind makes nano titanium oxide uniform in the polymer
The method of distribution.
Background technology
Now conventional inorganic nano antiseptic mainly has two kinds of Nano Silver and nano TiO 2.Nano titanium oxide can be except thin
Bacterium, purify air is because it under conditions of light or water, and the electronics in its valence band is excited to conduction band, produces in valence band
Hole, free electron-hole pair can make oxygen and water activation, produce and have the very active oxygen of high reaction activity and OH free radicals, right
Pernicious gas and bacterium in air has very strong degradation, so as to give the good antibiotic property of coating and purify air
Energy；Nano Silver is accomplishes nano level argent simple substance by particle diameter, and it is to the number such as Escherichia coli, gonococcus, chlamydia trachomatis
Ten kinds of pathogenic microorganisms have strong suppression and killing action, and will not produce drug resistance, thus can by its with polyethylene,
The blending of the materials such as polypropylene makes food packaging items.
Nano Silver and nano titanium oxide are combined, the antibiotic property of coating is can further improve.On the one hand, Nano Silver
Exist as impurity, the wide catalytic performance of nano titanium oxide can be strengthened；On the other hand, Nano Silver is slowly released
Ag+, can destroy the activity of protozoa organized enzyme, with very strong bactericidal properties, and not affected by external condition (Guang Heshui).
But because nano silver material belongs to metastable material, to environmental factors such as temperature, vibration, illumination, magnetic field and atmosphere
It is especially sensitive, it is possible to voluntarily to grow up at normal temperatures, there is easily reunion, oxidizable and other materials compound tense intermiscibility difference
Problem, this will prevent nano metal material proper property from substantially or completely being played.By nano titanium oxide and Nano Silver
Mixing material be used in the polymer such as the materials such as polyethylene, polypropylene or polyvinyl chloride, its in Blending Processes easily
Reunite, so as to the material property for causing Nano Silver and nano titanium oxide can not be not fully exerted.
The content of the invention
Present disclosure is to provide one kind and makes nano titanium oxide equally distributed method in the polymer, its can gram
Take certain or some defects of prior art.
One kind proposed by the present invention makes nano titanium oxide equally distributed method in the polymer, and it includes following step
Suddenly：
Step (1)：Prepare Nano Silver；
Step (2)：Prepare nano titanium oxide；
Step (3)：By nano titanium oxide surface of the nano-silver loaded in step (1) in step (2), nanometer is obtained
TiO 2 carrying silver composite material；
Step (4)：Film forming agent, defoamer, levelling are added in the nano TiO 2 carrying silver composite material of step (3)
Agent；
Step (5)：The mixture that step (4) is obtained is evenly mixed in polymer.
Preferably, step (1) specifically includes following steps：
Step 1.1：Silver ammino solution of the silver nitrate content for 20-100g/L is equipped with, polyethylene pyrrole is added in silver ammino solution
Pyrrolidone, polyvinyl alcohol form composite solution, and the weight ratio of wherein silver ammino solution, polyvinylpyrrolidone and polyvinyl alcohol is
4:3:2；
Step 1.2：Crown ether is added in the composite solution of step 1.1, crown ether weight ratio is the 40-50% of composite solution；
Step 1.3：Add weight ratio for the 30% of composite solution sodium citrate in the composite solution of step 1.2, obtain
To Nano silver solution；
Step 1.4：The weight ratio added in step 1.3 Nano silver solution is the agar of the 40% of Nano silver solution, and
3-4 times of deionized water for adding weight ratio to be agar quality, is sufficiently mixed, and forms pasty state Nano Silver；
Step 1.5：The pasty state Nano Silver formed in step 1.4 is first freezed into 0.5h at a temperature of -10 DEG C, then in room
Middle benefit gas place 2h, then 10-20min is placed at a temperature of 70-80 DEG C；
Step 1.6：Nanometer galactic longitude ultraviolet irradiation 20-25min after step 1.5 is processed, obtains nano silver colloidal sol；
Step 1.7：Mercaptan and starch are added in the nano silver colloidal sol that step 1.6 is obtained, mixture is made in ultrasonic wavelength-division
Under dissipating effect, stir, wherein the weight ratio of nano silver colloidal sol, mercaptan and starch is 3:2:1；
Mixture after step 1.8 stirs step 1.7 seals lucifuge and places in temperature is for 10-15 DEG C of environment
Jing centrifugations, vacuum drying, grinding after 45-60 days obtains Nano Silver powder.
Nano Silver is obtained using said method, it first passes through crown ether in preparation process, first before reducing nano-silver
And sodium citrate, sodium citrate makes crown ether and alkali metal ion form stable complex as containing alkali-metal reducing agent,
The distance between positive and negative charge in Nano Silver system is pulled open, so as to realize the pretreatment to Nano silver solution so as to dispersive property
Improve, reduce agglomeration.Then reductive monosaccharide is generated as by agar homogeneous hydrolysis, realizes homogeneous controllable Nano Silver also
It is primary into while so that agar serves as the protective agent of Nano Silver, preventing the reunion of Nano Silver, gained Nano Silver is well dispersed, grain
Sub- shape is regular, and the Nano Silver after by reduction is through low temperature, high-temperature-phase after process so as to which internal structure tissue is disperseed,
Destroy its reunion performance；Finally nano silver colloidal sol is obtained after irradiating through ultraviolet, and sulphur is added in nano silver colloidal sol
Alcohol and starch so as to which surface forms nonpolar group, and prevents silver nano-grain movement to a certain extent, to ensure poly-
After being sufficiently mixed in compound, Nano Silver can uniformly mix, and be less prone to reunion, deposited phenomenon.
Preferably, step (2) specifically includes following steps：
Step 2.1, by concentration for 0.5mol/L titanyl sulfate solution and 5mol/L sodium hydroxide solution mixing, obtain
Nano-TiO 2 precursor；
Step 2.2, by nano-TiO 2 precursor at a temperature of 250 DEG C hydro-thermal reaction 10h, be subsequently cooled to room temperature；
Add weight ratio newborn for the acrylate of mixed liquor 15% in step 2.3, the mixed liquor in step 2.2 after cooling
Liquid, then filters, washs, is vacuum dried, and obtains nano-titanium dioxide powder；By acrylic acid ester emulsion and nano titanium oxide
The acidic surface of presoma is combined, and nano titanium oxide is uniformly divided by sterically hindered effect and Coulomb repulsion stabilization
Dissipate, and keep the long-time stability of mixed liquor.
Weight ratio is added to be 5 times of titanium dioxide powder in step 2.4, the nano-titanium dioxide powder for obtaining step 2.3
Methyl alcohol, obtain mixed liquor；
Step 2.5, in the mixed liquor of step 2.4 weight ratio is added for the nonionic surfactant of mixed liquor 10%；
It is soaked by adding methyl alcohol in nano-titanium dioxide powder, then improves nano-silica using nonionic surfactant
Change the chemical property of titanium so as to lipophile, low polarity, low-surface-energy, be difficult to reunite and the application such as dispersed
Characteristic so as to dispersed and be compound in polymer with nanoscale, prepares with nano titanium oxide work(
The composite of energy property.
Step 2.6, add NaOH that concentration is 30% and adjust PH=8, then by ultrasonically treated so as to uniform point
Dissipate, obtain modified nano titanium oxide.PH is adjusted by NaOH so as to which PH is higher, so that suspension system is away from two
The isoelectric point of titanium oxide, electrostatic repulsion forces effect each other increases, and making the stability of system increases.
Preferably, in step 1.8 at 80～100 DEG C be vacuum dried 4～6h；It is true at 40～60 DEG C in step 2.3
Sky is dried 2～3h.
Preferably, ultrasonically treated in step 1.7 is to use 150r/ in operating frequency is for the ultrasonic reaction kettle of 30-40kHz
The stirring at low speed of min.
Preferably, polymer is polyethylene, polypropylene or polyvinyl chloride in step 1.9.
Specific embodiment
To further appreciate that present disclosure, in conjunction with the embodiments the present invention is described in detail.It should be appreciated that real
Apply example be only the present invention is explained and and it is non-limiting.
Embodiment 1
One kind makes nano titanium oxide equally distributed method in the polymer, and it is comprised the following steps：
Step (1)：Prepare Nano Silver；
Step (2)：Prepare nano titanium oxide；
Step (3)：By nano titanium oxide surface of the nano-silver loaded in step (1) in step (2), nanometer is obtained
TiO 2 carrying silver composite material；
Step (4)：Film forming agent, defoamer, levelling are added in the nano TiO 2 carrying silver composite material of step (3)
Agent；Common auxiliary agent on the market that film forming agent, defoamer, levelling agent are adopted.
Step (5)：The mixture that step (4) is obtained is evenly mixed in polymer.
Wherein, step (1) specifically includes following steps：
Step 1.1：Silver ammino solution of the silver nitrate content for 20-100g/L is equipped with, polyethylene pyrrole is added in silver ammino solution
Pyrrolidone, polyvinyl alcohol form composite solution, and the weight ratio of wherein silver ammino solution, polyvinylpyrrolidone and polyvinyl alcohol is
4:3:2；Polyvinylpyrrolidone and polyethylene were added in silver ammino solution before silver ammino solution is reduced into into Nano silver solution
Alcohol, makes silver ion be surrounded by polyvinylpyrrolidone, and separated by the long-chain of polyvinylpyrrolidone, it is to avoid silver nano-grain
Coagulation, while particle size of the polyvinylpyrrolidone as surfactant energy effective control Nano Silver, so as to play effectively
Prevent nano-Ag particles from reuniting.
Step 1.2：Crown ether is added in the composite solution of step 1.1, crown ether weight ratio is the 40-50% of composite solution；
Step 1.3：Add weight ratio for the 30% of composite solution sodium citrate in the composite solution of step 1.2, obtain
To Nano silver solution；
Crown ether is added in composite solution in step 1.2 and step (3).Crown ether has hydrophobic external skeletal and hydrophilic
, while stable complex can also be formed with sodium citrate, reactant can be on the one hand made with the inner chamber of metal ion bonding
Reduction anion dissociate in system or exposed has higher reactivity, and alkali metal cation can also on the other hand be preced with
Ether is coated in inner chamber, thus just pulls open the distance between positive and negative charge in Nano Silver system so that Nano Silver can stably divide
Dissipate in the aqueous solution, be difficult to reunite, it is easy to preserve.
Step 1.4：The weight ratio added in step 1.3 Nano silver solution is the agar of the 40% of Nano silver solution, and
3-4 times of deionized water for adding weight ratio to be agar quality, is sufficiently mixed, and forms pasty state Nano Silver；Agar potentially acts as nanometer
The protective agent of silver, prevents the reunion of Nano Silver, further improves the dispersive property of Nano Silver, and makes nano silver particles shape more
Plus it is regular.
Step 1.5：The pasty state Nano Silver formed in step 1.4 is first freezed into 0.5h at a temperature of -10 DEG C, then in room
Middle benefit gas place 2h, then 10-20min is placed at a temperature of 70-80 DEG C；First freezed by pasty state Nano Silver so as to internal structure
Certain dispersion is obtained, then is stood at room temperature, be then dried in the higher environment of relative room temperature, so that in Nano Silver
Portion's chemistry tissue produces change, and dispersive property is further enhanced.
Step 1.6：Nanometer galactic longitude ultraviolet irradiation 20-25min after step 1.5 is processed, obtains nano silver colloidal sol；
Step 1.7：Mercaptan and starch are added in the nano silver colloidal sol that step 1.6 is obtained, mixture is made in operating frequency
It is uniform for the stirring at low speed in the ultrasonic reaction kettle of 30-40kHz with 150r/min, realize ultrasonic wave peptizaiton, wherein nanometer
The weight ratio of silver sol, mercaptan and starch is 3:2:1；
By Nano Silver under the action of uv light so as to ultimately form stable Nano silver solution, now its chemical property
It is held essentially constant, mercaptan and starch is now added in the solution so that sulfydryl reacts with Nano Silver, in nanometer silver surface shape
Into stable alkyl hydrosulfide silver phase, make nano-silver powder surface form nonpolar group, so as to improve the hydrophily of Nano Silver, carry
High modified Nano silver powder dispersibility in aqueous.And the starch for adding can increase reactant liquor viscosity, course of reaction is made
The silver nano-grain of middle generation is mobile restricted in reaction solution, so as to effectively suppress Nano Silver to reunite.
Mixture after step 1.8 stirs step 1.7 seals lucifuge and places in temperature is for 10-15 DEG C of environment
Jing centrifugations after 45-60 days, 4～6h, grinding are vacuum dried at 80～100 DEG C and obtain Nano Silver powder, through certain hour
Normal temperature and pressure avoid light place so that the Silver Clusters, silver ion, hydroxy, polyvinylpyrrolidone and polyethylene pyrrole in mixture
Cough up
Alkanone reaches dynamic equilibrium with the complex of silver in ratio, so as to be effectively improved obtained Nano Silver powdery
Can, strengthen its antibacterial, bactericidal property.
Step (2) specifically includes following steps：
Step 2.1, by concentration for 0.5mol/L titanyl sulfate solution and 5mol/L sodium hydroxide solution mixing, obtain
Nano-TiO 2 precursor；
Step 2.2, by nano-TiO 2 precursor at a temperature of 250 DEG C hydro-thermal reaction 10h, be subsequently cooled to room temperature；
Add weight ratio newborn for the acrylate of mixed liquor 15% in step 2.3, the mixed liquor in step 2.2 after cooling
Liquid, then filters, washing, is vacuum dried 2～3h at 40～60 DEG C, obtains nano-titanium dioxide powder；By acrylate breast
Liquid is combined with the acidic surface of nano-TiO 2 precursor, and by sterically hindered effect and Coulomb repulsion stabilization nanometer is made
Titanium dioxide is dispersed, and keeps the long-time stability of mixed liquor.
Weight ratio is added to be 5 times of titanium dioxide powder in step 2.4, the nano-titanium dioxide powder for obtaining step 2.3
Methyl alcohol, obtain mixed liquor；
Step 2.5, in the mixed liquor of step 2.4 weight ratio is added for the nonionic surfactant of mixed liquor 10%；
It is soaked by adding methyl alcohol in nano-titanium dioxide powder, then improves nano-silica using nonionic surfactant
Change the chemical property of titanium so as to lipophile, low polarity, low-surface-energy, be difficult to reunite and the application characteristic such as dispersed, make
It is dispersed with nanoscale and is compound in polymer, prepares the composite with nano titanium oxide functional.
Step 2.6, add NaOH that concentration is 30% and adjust PH=8, then by ultrasonically treated so as to uniform point
Dissipate, obtain modified nano titanium oxide.PH is adjusted by NaOH so as to which PH is higher, so that suspension system is away from two
The isoelectric point of titanium oxide, electrostatic repulsion forces effect each other increases, and making the stability of system increases.
It is demonstrated experimentally that be difficult to reunite when mixing in the polymer using the Nano Silver obtained by the technique in the present embodiment,
Good dispersion property, is supported on nano titanium oxide surface so that nano paint has a high-efficient and lasting anti-microbial property, and its
In nano titanium oxide it is dispersed and be compound in organic polymer with nanoscale, so as to prepare with nanometer two
The functional composite of titanium oxide.
Below schematically to the present invention and embodiments thereof be described, the description is not restricted.So, if
One of ordinary skill in the art is enlightened by it, in the case of without departing from the invention objective, without creatively designing
Go out the scheme and embodiment similar to the technical scheme, protection scope of the present invention all should be belonged to.
Claims (7)
1. one kind makes nano titanium oxide equally distributed method in the polymer, it is characterised in that it is comprised the following steps：
Step (1)：Prepare Nano Silver；
Step (2)：Prepare nano titanium oxide；
Step (3)：By nano titanium oxide surface of the nano-silver loaded in step (1) in step (2), nano-silica is obtained
Change titanium and carry silver composite material；
Step (4)：Film forming agent, defoamer, levelling agent are added in the nano TiO 2 carrying silver composite material of step (3)；
Step (5)：The mixture that step (4) is obtained is evenly mixed in polymer.
2. one kind according to claim 1 makes nano titanium oxide equally distributed method in the polymer, its feature exist
In：Step (1) specifically includes following steps：
Step 1.1, outfit silver nitrate content are the silver ammino solution of 20-100g/L, and polyvinylpyrrolidine is added in silver ammino solution
Ketone, polyvinyl alcohol form composite solution, and the wherein weight ratio of silver ammino solution, polyvinylpyrrolidone and polyvinyl alcohol is 4:3:
2, stand 24h after uniform mixing；
Step 1.2, add in the composite solution of step 1.1 crown ether, crown ether weight ratio for composite solution 40-50%；
Step 1.3,：Add weight ratio for the 30% of composite solution sodium citrate in the composite solution of step 1.2, received
The silver-colored solution of rice；
The agar of step 1.4,40% that the weight ratio added in step 1.3 Nano silver solution is Nano silver solution, and add
Weight ratio is 3-4 times of deionized water of agar quality, is sufficiently mixed, and forms pasty state Nano Silver；
Step 1.5, the pasty state Nano Silver formed in step 1.4 is first freezed into 0.5h at a temperature of -10 DEG C, then at room temperature
2h is placed, then 10-20min is placed at a temperature of 70-80 DEG C；
Step 1.6, step 1.5 is processed after nanometer galactic longitude ultraviolet irradiation 20-25min, obtain nano silver colloidal sol；
Step 1.7, mercaptan and silane coupler and starch containing sulfydryl are added in the nano silver colloidal sol that step 1.6 is obtained,
Make mixture under ultrasonic wave peptizaiton, stir, wherein the weight ratio of nano silver colloidal sol, mercaptan and starch is 3:2:
1；
Step 1.8, step 1.7 is stirred after mixture sealing lucifuge and place 45-60 in temperature is for 10-15 DEG C of environment
Jing centrifugations, vacuum drying, grinding after it obtains Nano Silver powder.
3. one kind according to claim 1 makes nano titanium oxide equally distributed method in the polymer, its feature exist
In：Step (2) specifically includes following steps：
Step 2.1, by concentration for 0.5mol/L titanyl sulfate solution and 5mol/L sodium hydroxide solution mixing, adjust PH=
7, obtain nano-TiO 2 precursor；
Step 2.2, by nano-TiO 2 precursor at a temperature of 250 DEG C hydro-thermal reaction 10h, be subsequently cooled to room temperature；
Weight ratio is added in step 2.3, the mixed liquor in step 2.2 after cooling for the acrylic acid ester emulsion of mixed liquor 15%,
Then filter, wash, be vacuum dried, obtain nano-titanium dioxide powder；
Add weight ratio for the methyl alcohol of 5 times of titanium dioxide powder in step 2.4, the titanium dioxide powder for obtaining step 2.3, obtain
To mixed liquor；
Step 2.5, in the mixed liquor of step 2.4 weight ratio is added for the nonionic surfactant of mixed liquor 10%；
Step 2.6, add NaOH that concentration is 30% and adjust PH=8, then by ultrasonically treated so as to it is dispersed,
Obtain modified nano titanium oxide.
4. one kind according to claim 2 makes nano titanium oxide equally distributed method in the polymer, its feature exist
In：In step 1.8 at 80～100 DEG C be vacuum dried 4～6h.
5. one kind according to claim 2 makes nano titanium oxide equally distributed method in the polymer, its feature exist
In：In step 2.3 at 40～60 DEG C be vacuum dried 2～3h.
6. one kind according to claim 2 makes nano titanium oxide equally distributed method in the polymer, its feature exist
In：Ultrasonically treated in step 1.7 is with the stirring at low speed of 150r/min in operating frequency is for the ultrasonic reaction kettle of 30-40kHz.
7. one kind according to claim 1 makes nano titanium oxide equally distributed method in the polymer, its feature exist
In：Polymer includes polyethylene, polypropylene and polyvinyl chloride in step (5).
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107706481A (en) * | 2017-11-23 | 2018-02-16 | 成都新柯力化工科技有限公司 | A kind of method based on hollow microsphere solid phase recovery anode material of lithium battery |
| CN111657273A (en) * | 2020-06-19 | 2020-09-15 | 福建省凡通科技发展有限公司 | Nano-silver bactericidal composition for fresh flowers |
| CN113308003A (en) * | 2021-07-06 | 2021-08-27 | 中国人民解放军63919部队 | Antibacterial nano composite film and preparation method thereof |
| CN117511056A (en) * | 2023-11-07 | 2024-02-06 | 贵州省纳米材料工程中心 | Polypropylene antibacterial material and preparation method thereof |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1830808A (en) * | 2006-03-28 | 2006-09-13 | 上海华明高技术（集团）有限公司 | Nanometer titanium dioxide water pulp and its preparation method |
| CN101596325A (en) * | 2009-07-08 | 2009-12-09 | 中国人民解放军第三军医大学野战外科研究所 | Nano-silver biological sponge and preparation method thereof |
| CN101654572A (en) * | 2008-08-22 | 2010-02-24 | 比亚迪股份有限公司 | Nano coating and preparation method thereof |
| CN102489717A (en) * | 2011-12-22 | 2012-06-13 | 云南云天化股份有限公司 | Preparation method of nanometer silver particles |
| CN103817321A (en) * | 2014-02-19 | 2014-05-28 | 南京林业大学 | Modified nano silver powder preparing method |
| CN103980738A (en) * | 2014-05-15 | 2014-08-13 | 北京化工大学 | Preparation method of coated modified nanometer titanium dioxide |
| CN104028779A (en) * | 2014-06-26 | 2014-09-10 | 淮阴工学院 | Semi-dry nano silver synthesis method |
-
2016
- 2016-11-24 CN CN201611041467.6A patent/CN106590060A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1830808A (en) * | 2006-03-28 | 2006-09-13 | 上海华明高技术（集团）有限公司 | Nanometer titanium dioxide water pulp and its preparation method |
| CN101654572A (en) * | 2008-08-22 | 2010-02-24 | 比亚迪股份有限公司 | Nano coating and preparation method thereof |
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