CN110170284A - A kind of super-hydrophobic TiO of response type2Microballoon and the preparation method and application thereof - Google Patents
A kind of super-hydrophobic TiO of response type2Microballoon and the preparation method and application thereof Download PDFInfo
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- CN110170284A CN110170284A CN201910368886.8A CN201910368886A CN110170284A CN 110170284 A CN110170284 A CN 110170284A CN 201910368886 A CN201910368886 A CN 201910368886A CN 110170284 A CN110170284 A CN 110170284A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/46—Oxides or hydroxides of elements of Groups 4 or 14 of the Periodic System; Titanates; Zirconates; Stannates; Plumbates
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/10—Repellency against liquids
- D06M2200/12—Hydrophobic properties
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/35—Abrasion, pilling or fibrillation resistance
Abstract
The present invention discloses a kind of super-hydrophobic TiO of response type2Microballoon and the preparation method and application thereof belongs to nano-macromolecule material field.It is to synthesize TiO by sol-gel method first2Colloidal sol hydrolyzes tetra-n-butyl titanate to prepare titanium colloidal sol using salt acid for adjusting pH value.The silane coupling agent with epoxy group is reused to TiO2It is modified, is assigning TiO2It while super-hydrophobic effect, can also preferably be combined with fabric, there is excellent durability.The TiO with super-hydrophobicity2The preparation method simple process of microballoon has potential using value preparing hydrophobic fabric, leading sweat and the fields such as perspire.
Description
Technical field
The invention belongs to nano-macromolecule material fields, and in particular to a kind of super-hydrophobic TiO of response type2Microballoon and its preparation
Method and application.
Background technique
Now in daily life metal oxide using more and more extensive, especially in catalytic field.Metal oxide
It is very important class catalyst, the research of metal oxide is unfolded extensively now and develops and is applied to all trades and professions,
And after oxidizing metal object nanosizing, obtain more excellent catalytic performance, it is contemplated that the important development side of catalyst
To will be research to metal oxide.
In Multimetal oxide, nano-TiO2Function admirable, be can be widely applied to it is important in daily life
Material.Nano-TiO2Outstanding advantages have: it is at low cost, efficient, energy saving, cleaning is nontoxic, thorough to organic matter degradation, stability is good
Well and there are unique optical physics and photochemical properties etc., these features make TiO2Become important research object, by wide
General concern.
But titanium dioxide itself has hydrophily, and when it arranges fabric, is only simply attached to fabric
Surface, therefore its rub resistance durability is poor, and when by strong friction, nano particle is easily fallen, and performance is caused to decline.
Therefore when preparing titanium dioxide using sol-gel method, using with hydrophobic effect and the combination that can react with fabric
Silane coupling agent TiO 2 sol is modified, make it have super-hydrophobicity and can have preferable in conjunction with fabric
Durable rub resistance effect.
Summary of the invention
Goal of the invention: the technical problem to be solved in the present invention is to provide a kind of super-hydrophobicities with preferable durable rub resistance
Nanometer titanium dioxide micro-sphere.
The present invention also technical problems to be solved are to provide the preparation method of above-mentioned super-hydrophobic nano titanium dioxide microballoon sphere.
The last technical problems to be solved of the present invention are to provide above-mentioned super-hydrophobicity nanometer titanium dioxide micro-sphere in the fabric
Application.
In order to solve the above technical problems, the present invention adopts the following technical scheme:
A kind of super-hydrophobic TiO of response type2The preparation method of microballoon, comprising the following steps:
(1) tetra-n-butyl titanate is added to absolute ethanol, is uniformly mixed；
(2) under agitation, the tetra-n-butyl titanate mixture that step (1) obtains is added drop-wise to simultaneously with hydrochloric acid solution
In ethanol water, adjusting pH with ammonium hydroxide is 2~4, obtains TiO 2 sol；
(3) under agitation, hydrophobictype silanes coupling agent is added into TiO 2 sol, adds oxygen-containing fundamental mode silicon
Alkane coupling agent, obtains modified titanium dioxide sol,
The hydrophobic silane coupling agent is methyltriethoxysilane (MTES), γ-chloropropyl triethoxysilane
(CPTS), the mixing of one or more of octyltri-ethoxysilane (OTES), dodecyl triethoxysilane (DTEOS)
The mixing of one or both of object, preferably methyltriethoxysilane (MTES), dodecyl triethoxysilane (DTEOS)
Object；
The silane coupling agent of the fundamental mode containing epoxy is γ-glycidyl ether oxygen propyl trimethoxy silicane (KH560)；
(4) it is centrifuged modified titanium dioxide sol, is washed, drying obtains modifying titanium dioxide blocks of solid, milled processed,
Obtain the super-hydrophobic TiO of response type2Microballoon.
The present invention is when preparing TiO 2 sol, by controlling the hydrolysis rate of tetra-n-butyl titanate to control titanium dioxide
The throughput rate and its particle size of titanium guarantee that the temperature of its hydrolysis rate, control synthesis of titanium dioxide particle diameter distribution are uniform.Benefit
TiO 2 sol is modified with the react silane coupling agent of combination of fabric, is grafted Long carbon chain on the titanium dioxide
With epoxy group, so that titanium dioxide has hydrophobicity and reactivity, and titanium dioxide microballoon sphere can be largely improved
Durable rub resistance.
In step (1), the mass ratio of the tetra-n-butyl titanate and dehydrated alcohol is 4~5:1, preferably 4:1.
In step (2), the concentration of hydrochloric acid is 1~2mol/L, preferably 1mol/L in the hydrochloric acid solution；The concentration of ammonium hydroxide is
1~2mol/L, preferably 1mol/L.
In step (2), the hydrochloric acid of addition and the mass ratio of tetra-n-butyl titanate are 3.5~4:1, preferably 4:1；Ethyl alcohol is water-soluble
The concentration of ethyl alcohol is 50% in liquid, tetra-n-butyl titanate mixture: the volume ratio of hydrochloric acid solution is 1:10~12, preferably 1:10；
Tetra-n-butyl titanate mixture: the volume ratio of ethanol solution is 2.5~3.5:1, preferably 3:1.
In step (2), the rate of addition of the tetra-n-butyl titanate mixture is 1~3 drop/s, speed of agitator is 350~
450r/min, reaction time are 2~4h.
In step (3), the mass ratio of the hydrophobictype silanes coupling agent and TiO 2 sol is 10-12:1, preferably 10:
1；The mass ratio of the oxygen-containing fundamental mode silane coupling agent and TiO 2 sol is 10-12:1, preferably 10:1.
In step (3), hydrophobictype silanes coupling agent, the silane coupling agent of fundamental mode containing epoxy are with TiO 2 sol when reacting
Between be 3~6h.
In step (3), hydrophobictype silanes coupling agent, the silane coupling agent of fundamental mode containing epoxy react temperature with TiO 2 sol
Degree is 10~40 DEG C.
In step (4), the super-hydrophobic TiO of response type2The partial size of microballoon is 200~300nm.
In step (4), the revolving speed of centrifuge is 6000~7000r/min, and centrifugation time is 10~25min.
In step (4), the drying temperature of titanium dioxide is 60~80 DEG C, and drying time is 40~60min.
Hydrolysis in the present invention using tetra-n-butyl titanate prepares modifying titanium dioxide gel, and speed is added dropwise by control
Degree controls the generating rate and partial size of titanium dioxide with content, and using the silane coupling agent with Long carbon chain to titanium dioxide
Titanium colloidal sol is modified, and in the presence of water, the methoxyl group in silane coupling agent can have an effect with hydrone, hydrolysis
Silicone hydroxyl is generated, can occur to shrink with the hydroxyl contained by titanium dioxide surface and react, so that silane coupling agent is grafted
Onto titanium dioxide, its excellent hydrophobic effect is assigned.And the silane coupling agent of the fundamental mode containing epoxy such as KH560, contained by
Epoxy group, the group that open loop and surface of cotton fabric can occur reacts, thus with the stronger combination of cotton fabric one
It rises, makes it have good durable crocking resistance.
The reaction mechanism is as follows with titanium dioxide for silane coupling agent:
The reaction mechanism is as follows for silane coupling agent and fabric with epoxy group:
TiO when silane coupling agent is added in titanium dioxide, with titanium dioxide surface2- OH reacts, to two
Titanium oxide realizes graft modification, to obtain super-hydrophobic titanium dioxide nanoparticle.The ring introduced simultaneously by silane coupling agent
When arranging to fabric, with the group of fabric surface ring-opening reaction occurs for oxygroup, thus be preferably combined together with fabric,
With excellent rub resistance endurance quality.
The utility model has the advantages that
The invention discloses a kind of preparation methods of hydrophobic microballoon of response type TiO2, prepare dioxy using sol-gel method
Change titanium colloidal sol, and control rate of addition controls hydrolysis rate with dripping quantity during the reaction, it is uniform to prepare particle diameter distribution
TiO 2 sol.It reuses silane coupling agent and graft modification is carried out to titanium dioxide, utilize what is contained in silane coupling agent
Long carbon chain and epoxy group assign the excellent super-hydrophobicity of titanium dioxide and can be with the performance of cotton fabric reaction bonded.
Preparation process of the invention is simple, cheap using reagent cost, is suitable for most techniques.It can be with after arrangement
Fabric ultra-hydrophobicity is assigned, and also there is excellent rub resistance endurance quality, even if titanium dioxide granule is by biggish
Friction, which will not be fallen, waits disrepair phenomenons, extends the service life of product.
Detailed description of the invention
1 titanium dioxide microballoon sphere emulsion particle diameter of Fig. 1 embodiment.
1 titanium dioxide microballoon sphere contact angle of Fig. 2 embodiment.
2 titanium dioxide microballoon sphere emulsion particle diameter of Fig. 3 embodiment.
2 titanium dioxide microballoon sphere contact angle of Fig. 4 embodiment.
3 titanium dioxide microballoon sphere emulsion particle diameter of Fig. 5 embodiment.
3 titanium dioxide microballoon sphere contact angle of Fig. 6 embodiment.
Specific embodiment
Below with reference to concrete mode, invention is further explained:
Embodiment 1:
(1) prepared by hydridization titanium colloidal sol: weighing 150.0g hydrochloric acid (1mol/L) and 55.0g deionized water, mixing is made into component
A；80.0g tetra-n-butyl titanate and 20.0g dehydrated alcohol are weighed, component B is made into uniformly with 150r/min mechanical stirring 3min；
(2) component B and component A being added dropwise in ethanol solution simultaneously under the conditions of 25 DEG C of room temperature, rate of addition is 2 drops/sec,
Titanium colloidal sol is prepared, until component A and B are added completely into 100.0g ethanol water；
(3) ammonium hydroxide (1mol/L) regulation system pH to 4 is added dropwise；
(4) 100mL TiO 2 sol is measured at 25 DEG C, is added 4mL octyltri-ethoxysilane (OTES), reaction
4h；4mL γ-glycidyl ether oxygen propyl trimethoxy silicane (KH560) is added, 4h is reacted, with the tachogenerator of 500r/min
Tool stirring, completes the modification to titanium dioxide；
(5) by titanium colloidal sol using centrifuge to be centrifuged 10min under the action of 1000r/min；Solid liquid phase is separated, by acquisition
It is dried 3 hours in the baking oven of 70 DEG C of colloid placement；It is milled into using alms bowl stick careful powdered.
Embodiment 2:
(1) prepared by hydridization titanium colloidal sol: weighing 150.0g hydrochloric acid (1mol/L) and 55.0g deionized water, mixing is made into component
A；80.0g tetra-n-butyl titanate and 20.0g dehydrated alcohol are weighed, component B is made into uniformly with 150r/min mechanical stirring 3min；
(2) component B and component A being added dropwise in ethanol solution simultaneously under the conditions of 25 DEG C of room temperature, rate of addition is 2 drops/sec,
Titanium colloidal sol is prepared, until component A and B are added completely into 100.0g ethanol water；
(3) ammonium hydroxide (1mol/L) regulation system pH to 4 is added dropwise；
(4) at 25 DEG C measure 100mL TiO 2 sol, be added 2mL dodecyl triethoxysilane (DTEOS) with
2mL γ-chloropropyl triethoxysilane (CPTS) mixture reacts 4h；Add 4mL γ-glycidyl ether oxygen propyl three
Methoxy silane (KH560) reacts 4h, with the revolving speed mechanical stirring of 500r/min, completes the modification to titanium dioxide；
(5) by titanium colloidal sol using centrifuge to be centrifuged 10min under the action of 1000r/min；Solid liquid phase is separated, by acquisition
It is dried 3 hours in the baking oven of 70 DEG C of colloid placement；It is milled into using alms bowl stick careful powdered.
Embodiment 3:
(1) prepared by hydridization titanium colloidal sol: weighing 150.0g hydrochloric acid (1mol/L) and 55.0g deionized water, mixing is made into component
A；80.0g tetra-n-butyl titanate and 20.0g dehydrated alcohol are weighed, component B is made into uniformly with 150r/min mechanical stirring 3min；
(2) component B and component A being added dropwise in ethanol solution simultaneously under the conditions of 25 DEG C of room temperature, rate of addition is 2 drops/sec,
Titanium colloidal sol is prepared, until component A and B are added completely into 100.0g ethanol water；
(3) ammonium hydroxide (1mol/L) regulation system pH to 4 is added dropwise；
(4) 100mL titanium colloidal sol is measured at 25 DEG C, is added 4mL methyltriethoxysilane (MTES), and 4h is reacted；Again plus
Enter 4mL γ-glycidyl ether oxygen propyl trimethoxy silicane (KH560), reacts 4h, with the revolving speed mechanical stirring of 500r/min,
Complete the modification to titanium dioxide；
(5) by titanium colloidal sol using centrifuge to be centrifuged 10min under the action of 1000r/min；Solid liquid phase is separated, by acquisition
It is dried 3 hours in the baking oven of 70 DEG C of colloid placement；It is milled into using alms bowl stick careful powdered.
The response type super dewatering titanium oxide microballoon powder prepared under the conditions of different hydrophobic silane coupling agents in embodiment
The performance at end, the titanium dioxide microballoon sphere that wherein prepared by case 1 is best, and milky is presented in color, and powder diameter is evenly distributed, can
To observe tiny titanium dioxide microballoon sphere under Electronic Speculum.Modified titanium dioxide microballoon sphere powder is pressed on glass slide
Piece, then the hydrophobic angle after tabletting is tested under DSA100 liquid drop analyzer, average hydrophobicity angle can achieve 150.81 °.By this
Kind response type super dewatering titanium oxide microsphere powder is scattered in reagent to react with fabric, contains in modifying titanium dioxide microballoon
Ring-opening reaction occurs for-the OH in some epoxy groups and cotton fabric, is combined together with fabric, so that super dewatering titanium oxide microballoon
Fastness to rubbing is excellent, after tested, after high-intensitive friction, still keeps its ultra-hydrophobicity.
Claims (10)
1. a kind of super-hydrophobic TiO of response type2The preparation method of microballoon, which comprises the following steps:
(1) tetra-n-butyl titanate is added to absolute ethanol, is uniformly mixed；
(2) under agitation, tetra-n-butyl titanate mixture and hydrochloric acid solution that step (1) obtains are added drop-wise to ethyl alcohol simultaneously
In aqueous solution, adjusting pH with ammonium hydroxide is 2~4, obtains TiO 2 sol；
(3) under agitation, hydrophobictype silanes coupling agent is added into TiO 2 sol, it is even to add oxygen-containing fundamental mode silane
Join agent, obtain modified titanium dioxide sol,
The hydrophobic silane coupling agent is methyltriethoxysilane, γ-chloropropyl triethoxysilane, three ethoxy of octyl
The mixture of one or more of base silane, dodecyl triethoxysilane,
The silane coupling agent of the fundamental mode containing epoxy is γ-glycidyl ether oxygen propyl trimethoxy silicane；
(4) it is centrifuged modified titanium dioxide sol, is washed, drying obtains modifying titanium dioxide blocks of solid, milled processed obtains
The super-hydrophobic TiO of response type2Microballoon.
2. the super-hydrophobic TiO of response type according to claim 12The preparation method of microballoon, which is characterized in that in step (1),
The mass ratio of the tetra-n-butyl titanate and dehydrated alcohol is 4~5:1.
3. the super-hydrophobic TiO of response type according to claim 12The preparation method of microballoon, which is characterized in that in step (2),
The concentration of hydrochloric acid is 1~2mol/L in the hydrochloric acid solution；The concentration of ammonium hydroxide is 1~2mol/L.
4. the super-hydrophobic TiO of response type according to claim 12The preparation method of microballoon, which is characterized in that in step (2),
The hydrochloric acid of addition and the mass ratio of tetra-n-butyl titanate are 3.5~4:1, the volume-fraction concentration of ethyl alcohol in the ethanol water
50%, tetra-n-butyl titanate mixture, hydrochloric acid solution volume ratio be 1:10~12, tetra-n-butyl titanate mixture, ethyl alcohol
The volume ratio of aqueous solution is 2.5~3.5:1.
5. the super-hydrophobic TiO of response type according to claim 12The preparation method of microballoon, which is characterized in that in step (2),
The rate of addition of the tetra-n-butyl titanate mixture is 1~3 drop/s, and speed of agitator is 350~450r/min, and the reaction time is
2~4h.
6. the super-hydrophobic TiO of response type according to claim 12The preparation method of microballoon, which is characterized in that in step (3),
The mass ratio of the hydrophobictype silanes coupling agent and TiO 2 sol be 10~12:1, the oxygen-containing fundamental mode silane coupling agent with
The mass ratio of TiO 2 sol is 10~12:1.
7. the super-hydrophobic TiO of response type according to claim 12The preparation method of microballoon, which is characterized in that in step (3),
The reaction time of hydrophobictype silanes coupling agent, the silane coupling agent of fundamental mode containing epoxy and TiO 2 sol is 3~6h；
In step (3), the reaction temperature of hydrophobictype silanes coupling agent, the silane coupling agent of fundamental mode containing epoxy and TiO 2 sol is equal
It is 10~40 DEG C
8. the super-hydrophobic TiO of response type according to claim 12The preparation method of microballoon, which is characterized in that in step (4),
The super-hydrophobic TiO of response type2The partial size of microballoon is 200~300nm.
9. any super-hydrophobic TiO of response type of claim 1~82The response type that the preparation method of microballoon is prepared is super-hydrophobic
TiO2Microballoon.
10. the super-hydrophobic TiO of response type described in claim 92Application of the microballoon in textile finishing.
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| CN111441166A (en) * | 2020-04-02 | 2020-07-24 | 海泰纺织（苏州）有限公司 | Oil-water separation fabric and preparation method thereof |
| CN112724720A (en) * | 2020-12-23 | 2021-04-30 | 江苏永阳新材料科技有限公司 | Water-based environment-friendly inorganic paint for interior walls and preparation method thereof |
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| WO2022147860A1 (en) * | 2021-01-06 | 2022-07-14 | 安徽工业大学 | Method for preparing superhydrophobic filter material of bag-type dust collector and use thereof |
| CN115182169A (en) * | 2022-06-29 | 2022-10-14 | 浙江科峰有机硅股份有限公司 | Special hydrophilic silicone oil and preparation method thereof |
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| CN111441166A (en) * | 2020-04-02 | 2020-07-24 | 海泰纺织（苏州）有限公司 | Oil-water separation fabric and preparation method thereof |
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| CN112941933A (en) * | 2021-02-04 | 2021-06-11 | 郑州市娅丽达服饰有限公司 | Fabric with visible and invisible patterns, garment designed and processed by fabric and processing method |
| CN112941933B (en) * | 2021-02-04 | 2023-04-11 | 郑州市娅丽达服饰有限公司 | Fabric with visible and invisible patterns, garment designed and processed by fabric and processing method |
| CN115182169A (en) * | 2022-06-29 | 2022-10-14 | 浙江科峰有机硅股份有限公司 | Special hydrophilic silicone oil and preparation method thereof |
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