CN106752113A - A kind of preparation method of modifying titanium dioxide and application - Google Patents
A kind of preparation method of modifying titanium dioxide and application Download PDFInfo
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- CN106752113A CN106752113A CN201611155302.1A CN201611155302A CN106752113A CN 106752113 A CN106752113 A CN 106752113A CN 201611155302 A CN201611155302 A CN 201611155302A CN 106752113 A CN106752113 A CN 106752113A
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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
- C09C1/3607—Titanium dioxide
- C09C1/3676—Treatment with macro-molecular organic compounds
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
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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
- C09C1/3607—Titanium dioxide
- C09C1/3615—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
- C09C1/3623—Grinding
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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
- C09C1/3607—Titanium dioxide
- C09C1/3615—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
- C09C1/363—Drying, calcination
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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
- C09C1/3607—Titanium dioxide
- C09C1/3653—Treatment with inorganic compounds
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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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- 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
- C09C3/066—Treatment or coating resulting in a free metal containing surface-region
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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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- General Health & Medical Sciences (AREA)
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Abstract
The present invention relates to polyester modification technical field, exist to solve current titanium dioxide and disperse in the melt irregular, photocatalytic degradation reaction easily occurs, the problems such as function is more single, the present invention proposes a kind of modifying titanium dioxide and preparation method thereof：By the reduction of the dipping, nano-Ag particles of titanium dioxide, titanium dioxide powder surface coating modification step, preparation method is relatively simple, and modified titanium dioxide has the low advantage of antibacterial functions, changeable colour, good dispersion, photocatalytic activity.
Description
Technical field
It is a kind of preparation side of new terylene modifying titanium dioxide specifically the present invention relates to technical field of modification
Method.
Background technology
Titanium dioxide is important chemical fibre delustering agent, typically there is three kinds of crystalline phases：Brockite, rutile and Anatase.
Wherein, brookite is in transitional face, it is difficult to obtain；Rutile Type hardness is higher, and abrasion is easily caused to filament spinning component, so that
The life-span of influence equipment and the quality of spinning；Anatase phase titanium dioxide source relative abundance, property are stablized, and are with it relatively
Fiber obtained in delustering agent is similar with natural fiber opacity, therefore current delustering agent is based on anatase titanium dioxide,
But there is also disperseing irregular in the melt, easily there is photocatalytic degradation reaction, the problems such as function is more single, this is just to two
The production of titanium oxide is prepared and modification technology proposes requirement higher.
At present, frequently with the modified mode in surface to improve the dispersiveness of titanium dioxide powder, and its photocatalysis work is reduced
Property etc., such as Application No. 201510669822.3 uses 2,2- dihydromethyl propionic acids in alcohols solvent system, after calcining
Nano titanium oxide is modified, and improves dispersiveness of the titanium dioxide in polymeric matrix, reduces its photocatalytic activity.
The content of the invention
Existing to solve current titanium dioxide disperse in the melt irregular, and photocatalytic degradation reaction easily occurs, function compared with
For it is single the problems such as, the present invention proposes a kind of modifying titanium dioxide and preparation method thereof, and preparation method is relatively simple, modified
Titanium dioxide there is the low advantage of antibacterial functions, changeable colour, good dispersion, photocatalytic activity.
It is also proposed application of the modified titanium dioxide in terylene simultaneously.
The present invention is achieved by the following technical solutions：A kind of preparation method of modifying titanium dioxide is following steps：
（1）The dipping of titanium dioxide
Filtered after titanium dioxide powder is impregnated into 15-30 min in the ethanol solution of silver nitrate, powder is dried；
Preferably, titanium dioxide powder is selected from anatase titanium dioxide powder, diameter of particle is 250-400 nm.Anatase
Type titanium dioxide source relative abundance, property are stablized relatively, and fiber obtained in it as delustering agent is opaque with natural fiber
Degree is similar
Preferably, the ethanol solution concentration of silver nitrate is 5-18 mmol/L, the mass content of titanium dioxide is in dipping system
5-20%, silver nitrate purity>99%, ethanol uses absolute ethyl alcohol.
Preferably, first stirring ultrasound again before impregnation, be conducive to being well mixed.
Preferably, being dried using vacuum drying oven.
（2）The reduction of nano-Ag particles
Powder after drying is processed into 12 more than h with ultraviolet lighting, until powder is presented taupe；
This is that the silver nitrate presoma on its surface is reduced into nano-Ag particles, and nano-Ag particles particle diameter is 15-20 nm, load
Quality is 0.1-0.5%.Nano-Ag particles have preferable anti-microbial property, and there is stronger electronics biography between titanium dioxide
The effect of passing, can influence the optical property of titanium dioxide.
Titanium dioxide powder colour developing is reversible in this step, after being developed the color through visible-light treatment, can be extensive through treatment with ultraviolet light again
Multiple taupe, after be in again corresponding color through panchromatic light or monochromatic light treatment.
（3）Titanium dioxide powder surface coating modification
By step（2）Ball milling after obtained powder, water, polyethylene glycol, auxiliary agent mixing, obtains modified after filtering, separation, drying
Titanium dioxide.
The usage amount of water is uniform to measure to make mixed liquor stabilization.
Preferably, powder is 9-499 with the mass ratio of polyethylene glycol:1, polyethylene glycol is used for titanium dioxide surface bag
Cover.
Preferably, polyethylene glycol is 9-99 with the mass ratio of auxiliary agent:1.Described auxiliary agent includes dispersant and antioxygen
Agent, wherein, dispersant is 1-9 with the mass ratio of antioxidant:1.Dispersant is selected from charge modifiers, preferably hexa metaphosphoric acid
Sodium, antioxidant is selected from butylated hydroxy anisole.
Preferably, Ball-milling Time is 2-5 hours, Ball-milling Time is unsuitable long, serious through sedimentation removal reunion after ball milling
Particle.
Modified titanium dioxide through ultraviolet light process after be in taupe, then through panchromatic light process after it is white, or
In corresponding monochrome light color after monochromatic light treatment, while there are antibacterial functions, and dispersiveness is preferable in polyester fondant, light
Catalysis activity is relatively low.
Modified titania powder is again through wet ball grinding Surface coating polyethylene glycol improving it in polyester fondant
Dispersiveness.Therefore modifying titanium dioxide obtained in a kind of preparation method of modifying titanium dioxide of the present invention is on terylene
Application.The terylene of preparation has various functions such as antibacterial, the lower changeable colour of different light source irradiations, and after coated with polyethylene glycol
Dispersiveness is preferable in polyester fondant, while reducing the activity of its photocatalytic degradation PET molecules.
Compared with prior art, the beneficial effects of the invention are as follows：
（1）Preparation method is simple；
（2）Modified titanium dioxide has the low advantage of antibacterial functions, changeable colour, good dispersion, photocatalytic activity；
（3）Modified titania powder improves the dispersiveness in polyester fondant in terylene, reduces its photocatalysis
The activity of degraded PET molecules.
Specific embodiment
The present invention is described in further detail below by embodiment, it is noted that implementation of the invention is not limited to
In the following examples, any type of flexible and/or change made to the present invention falls within protection scope of the present invention
It is interior.
In the present invention, if not refering in particular to, all of ratio, percentage are unit of weight, all of raw material, equipment etc.
It is commercially available or the industry is conventional, wherein titanium dioxide, the purity of polyethylene glycol is equal>97%, the particle diameter of titanium dioxide exists
Between 250-400 nm.
Embodiment 1
18 mmol silver nitrates are added into 2 L（1578 g）Dissolved in ethanol solution, then by 220 g Detitanium-ore-type titanium dioxides
Titanium valve body is scattered in the ethanol solution of silver nitrate, ultrasonic 10 min after 10 min of stirring, then stands 15 min of dipping.Dipping
Titanium dioxide powder afterwards is separated by suction filtration, 30 DEG C of dryings of vacuum drying oven.Titanium dioxide powder ultraviolet lighting after drying
12 h are processed, taupe is presented to powder.The g of titanium dioxide powder 200, the g of polyethylene glycol 1, six inclined phosphorus of Argent grain will be loaded
The mg of sour sodium 15, the mg of butylated hydroxy anisole 5, mix with 200 g desalted waters, the h of ball milling 2, and sedimentation is removed reunites serious
Grain, suspension can obtain finally modified titanium dioxide powder 1 after being dried through the isolated titanium dioxide of suction filtration.
Embodiment 2
54 mmol silver nitrates are added into 6 L（4734 g）Dissolved in ethanol solution, then by 660 g Detitanium-ore-type titanium dioxides
Titanium valve body is scattered in the ethanol solution of silver nitrate, ultrasonic 20 min after 10 min of stirring, then stands 30 min of dipping.Dipping
Titanium dioxide powder afterwards is separated by suction filtration, 30 DEG C of dryings of vacuum drying oven.Titanium dioxide powder ultraviolet lighting after drying
18 h are processed, taupe is presented to powder.The g of titanium dioxide powder 600, the g of polyethylene glycol 50, six inclined phosphorus of Argent grain will be loaded
The g of sour sodium 0.255, the g of butylated hydroxy anisole 0.255, mix with 400 g desalted waters, the h of ball milling 3, and sedimentation is removed reunites seriously
Particle, suspension can obtain finally modified titanium dioxide powder 2 after being dried through the isolated titanium dioxide of suction filtration.
Embodiment 3
18 mmol silver nitrates are added into 2 L（1578 g）Dissolved in ethanol solution, then by 220 g Detitanium-ore-type titanium dioxides
Titanium valve body is scattered in the ethanol solution of silver nitrate, ultrasonic 10 min after 10 min of stirring, then stands 25 min of dipping.Dipping
Titanium dioxide powder afterwards is separated by suction filtration, 30 DEG C of dryings of vacuum drying oven.Titanium dioxide powder ultraviolet lighting after drying
15 h are processed, taupe is presented to powder.The g of titanium dioxide powder 200, the g of polyethylene glycol 5, six inclined phosphorus of Argent grain will be loaded
The g of sour sodium 0.234, the g of butylated hydroxy anisole 0.026, mix with 150 g desalted waters, the h of ball milling 2, and sedimentation is removed reunites seriously
Particle, suspension can obtain finally modified titanium dioxide powder 3 after being dried through the isolated titanium dioxide of suction filtration.
Application examples 1 ~ 3：
Modified titanium dioxide powder 1 ~ 3 and ethylene glycol co-formulation prepared by embodiment 1 ~ 3 into after slurry in the second ester
The change stage adds, and prepares omni-direction permutation section, and by obtaining delustring polyester fiber after spinning, after being processed through panchromatic light
It is white, also can again by treatment with ultraviolet light recover taupe, after again through panchromatic light or monochromatic light treatment be in other corresponding face
Color.
After long-time exposure experiments to light, the delustring polyester fiber of modified titanium dioxide powder its photocatalytic degradation feelings are added
Condition has been alleviated.
Claims (8)
1. a kind of preparation method of modifying titanium dioxide, it is characterised in that described preparation method is following steps：
（1）The dipping of titanium dioxide
Filtered after titanium dioxide powder is impregnated into 15-30 min in the ethanol solution of silver nitrate, powder is dried；
（2）The reduction of nano-Ag particles
Powder after drying is processed into 12 more than h with ultraviolet lighting, until powder is presented taupe；
（3）Titanium dioxide powder surface coating modification
By step（2）Ball milling after obtained powder, water, polyethylene glycol, auxiliary agent mixing, obtains modified after filtering, separation, drying
Titanium dioxide.
2. a kind of preparation method of modifying titanium dioxide according to claim 1, it is characterised in that step（1）Middle dioxy
Change titanium valve body and be selected from anatase titanium dioxide powder, diameter of particle is 250-400 nm.
3. a kind of preparation method of modifying titanium dioxide according to claim 1, it is characterised in that step（1）Middle nitric acid
The ethanol solution concentration of silver is 5-18 mmol/L, and the mass content of titanium dioxide is 5-20% in dipping system.
4. a kind of preparation method of modifying titanium dioxide according to claim 1, it is characterised in that step（3）Powder with
The mass ratio of polyethylene glycol is 9-499:1.
5. a kind of preparation method of the modifying titanium dioxide according to claim 1 or 4, it is characterised in that step（3）In gather
Ethylene glycol is 9-99 with auxiliary agent mass ratio:1.
6. the preparation method of a kind of modifying titanium dioxide according to claim 5, it is characterised in that described auxiliary agent is included
Dispersant and antioxidant, wherein, dispersant is 1-9 with the mass ratio of antioxidant:1.
7. the preparation method of a kind of modifying titanium dioxide according to claim 6, it is characterised in that dispersant is selected from electric charge
Modifying agent, antioxidant is selected from butylated hydroxy anisole.
8. modifying titanium dioxide obtained in a kind of a kind of preparation method of modifying titanium dioxide as claimed in claim 1 is in terylene
On application.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108384061A (en) * | 2018-01-31 | 2018-08-10 | 潍坊学院 | A kind of plastics heat-resisting composite light stabilizer and preparation method thereof |
| CN109896545A (en) * | 2019-03-14 | 2019-06-18 | 东北石油大学 | A kind of hollow shell-type titanium dioxide nano material, hollow shell-type titanium dioxide nano material of silver load and preparation method thereof |
| CN111014664A (en) * | 2019-11-19 | 2020-04-17 | 昆明理工大学 | Preparation method of antibacterial porous titanium alloy |
| CN111607837A (en) * | 2019-02-22 | 2020-09-01 | 南亚塑胶工业股份有限公司 | Recycled polyester fiber |
| CN111747743A (en) * | 2020-06-12 | 2020-10-09 | 广州凯立达电子股份有限公司 | Spherical piezoelectric ceramic and preparation method thereof |
| CN111995364A (en) * | 2020-08-25 | 2020-11-27 | 广东欧文莱陶瓷有限公司 | Antibacterial rock plate and preparation method thereof |
| CN112438274A (en) * | 2020-04-03 | 2021-03-05 | 祁海强 | Preparation method of high-dispersion anti-discoloration nano-silver antibacterial agent material |
| CN114836847A (en) * | 2022-04-07 | 2022-08-02 | 浙江恒逸石化研究院有限公司 | Bacteriostatic and delustering agent for chemical fibers and preparation method and application thereof |
| CN115093640A (en) * | 2022-07-30 | 2022-09-23 | 山东立卓睡眠科技有限公司 | Degradable PE fiber tube, preparation method and application of degradable PE fiber tube as pillow inner filler |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108384061A (en) * | 2018-01-31 | 2018-08-10 | 潍坊学院 | A kind of plastics heat-resisting composite light stabilizer and preparation method thereof |
| US11168198B2 (en) | 2019-02-22 | 2021-11-09 | Nan Ya Plastics Corporation | Recycled polyester fiber |
| CN111607837A (en) * | 2019-02-22 | 2020-09-01 | 南亚塑胶工业股份有限公司 | Recycled polyester fiber |
| CN111607837B (en) * | 2019-02-22 | 2022-12-20 | 南亚塑胶工业股份有限公司 | Recycled polyester fiber |
| TWI713998B (en) * | 2019-02-22 | 2020-12-21 | 南亞塑膠工業股份有限公司 | Preparation of a titanium dioxide-containing slurry and its application to recycled polyester fiber |
| CN109896545A (en) * | 2019-03-14 | 2019-06-18 | 东北石油大学 | A kind of hollow shell-type titanium dioxide nano material, hollow shell-type titanium dioxide nano material of silver load and preparation method thereof |
| CN109896545B (en) * | 2019-03-14 | 2021-08-20 | 东北石油大学 | Hollow shell type titanium dioxide nano material, silver-loaded hollow shell type titanium dioxide nano material and preparation method thereof |
| CN111014664A (en) * | 2019-11-19 | 2020-04-17 | 昆明理工大学 | Preparation method of antibacterial porous titanium alloy |
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