CN107675483A - A kind of preparation method of the titania nanotube based on click chemistry/bafta catalysis material - Google Patents
A kind of preparation method of the titania nanotube based on click chemistry/bafta catalysis material Download PDFInfo
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- CN107675483A CN107675483A CN201710860004.0A CN201710860004A CN107675483A CN 107675483 A CN107675483 A CN 107675483A CN 201710860004 A CN201710860004 A CN 201710860004A CN 107675483 A CN107675483 A CN 107675483A
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- 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
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- 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
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- 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
Abstract
The present invention relates to a kind of preparation method of the titania nanotube based on click chemistry/bafta catalysis material, synthesis including pre-processing bafta, reduce the synthesis of bafta, the synthesis of bromo Dopamine hydrochloride, the synthesis of bromo titania nanotube, the synthesis of the titania nanotube based on click chemistry/bafta catalysis material.The method of the present invention is simple, and cost is low, and mild condition, product yield high, side reaction is few, environmental protection；The titania nanotube based on click chemistry that the present invention is prepared/bafta catalysis material adsorption efficiency is high, stability is good, with good photocatalysis effect and the excellent feature of environmental protection, it can be used for the processing of dyestuff in dyeing waste water, widened application of the bafta in terms of waste water from dyestuff is adsorbed in photocatalysis.
Description
Technical field
The invention belongs to fabric modifying field, more particularly to a kind of titania nanotube/cotton based on click chemistry
The preparation method of fabric catalysis material.
Background technology
Functions of textile fabrics is the study hotspot of field of textiles in recent years, by introducing functional organic or inorganic nanometer
Structural material assigns fiber or the certain feature of textile, especially in the property such as photocatalysis, Degradation Formaldehyde, automatically cleaning, antibacterial
The research of energy aspect is quickly grown in recent years.Generally, the functionalization of textile can not only pass through emerging production technology and original
Material is made, but also can be realized by the new way of fabric modifying.By adding functional additive (organic or nothing
Machine nano structural material) modified textile is one of most important method.In numerous functional additives, a kind of photochemical catalyst
Light reaction and redox reaction can occur between its surface adsorbate in beche-de-mer without spike with, turn into functions of textile fabricsization research
In more promising material.
The new type functional material that catalysis material is potential very much as one kind, led in recent years as material science research
Heat subject in domain.For nano titanium oxide because size is small, specific surface area is big, the difference inside the key state and particle on surface,
Surface atom coordination is not congruent, causes the active position on surface to be increased, forms rough atomic stepses, increases reaction
Contact surface.Nano titanium dioxide photocatalysis technical matters is simple, and cost is cheap, at normal temperatures and pressures can oxidation Decomposition structure it is steady
Fixed organic matter, it is non-secondary pollution, nontoxic, nonirritant, heat-resist, thus photocatalysis is in fields such as processing waste gas, waste water
Have broad application prospects.Such as：The patent of Application No. 200910055165.8 discloses a kind of series modified nano two
Titanium dioxide photocatalyst fabric finishing agent and preparation method, it is by the way that modified nano-titanium dioxide colloidal sol and crosslinking agent are mixed
Series modified nano titanium dioxide photocatalyst finishing agent is obtained, other auxiliary agents and catalyst is added and is stirred and produce product.
The performance of textile photocatalytic degradation organic volatile is imparted after collated, it is multiple also to have UV resistance and antibacterial and mouldproof deodorization etc. concurrently
Close multi-functional.But there is preparation technology complexity, poor durability, light in modified nano-titanium dioxide Photo-Catalyst Fabric prepared by this method
The problems such as catalyst deteriorates fibrous material.Number of patent application 201210398660.0 discloses a kind of highlight catalytic active nano two
The method that titanium oxide polyester fiber is modified, the invention pass through directly in PET fiber surface loaded metal ion and doped anatase
Phase nano-titanium dioxide film so that modified polyester fiber not only has good photocatalysis efficiency while expands light
Response range is composed, and improves the self-cleaning ability of polyester fiber.But the highlight catalytic active nano prepared by this method
Titanium dioxide polyester fiber is with high costs, complex process, while the anatase-phase nano titanium dioxide adulterated is easily lost in, subsequently
Separate and reclaim and be relatively difficult.Number of patent application 201510756694.6 disclose it is a kind of be used for handle dyeing waste water fabric and
Its preparation method, it is characterised in that by one layer of nanometer titanium dioxide layer of dacron area load, increasing titanium dioxide
With the contact area of waste water, the efficiency of wastewater treatment is improved.But comparing distinct issues using fabric made from the technology is
Nano-titanium dioxide powder material is still easily reunited, and causes photocatalytic activity to reduce, and nano titanium oxide recovery is very
Difficulty is subject to certain restrictions its development.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of titania nanotube/bafta based on click chemistry
The preparation method of catalysis material, this method is simple, mild condition, the nano titania based on click chemistry being prepared
Pipe/bafta catalysis material adsorption efficiency is high.
A kind of preparation method of the titania nanotube based on click chemistry/bafta catalysis material of the present invention,
Comprise the following steps that:
(1) bafta is pre-processed, obtains pre-processing bafta；
(2) dissolve reduce agent in and reductant solution is formed in solvent, stir, the pretreatment bafta in step (1) is soaked
Enter in reductant solution, dry, obtain reducing bafta, the wherein concentration of reductant solution is 0.01-0.05g/ml, reducing agent
Mass ratio with pre-processing bafta is 1:1-3:1；
(3) titania nanotube is dissolved in solvent and forms solution, ultrasound, lucifuge stirring, add bromo hydrochloric acid DOPA
Amine, lucifuge continue to stir, and wash, and dry, obtain bromo titania nanotube, wherein titania nanotube solution concentration is
The mass ratio of 0.6-2.4mg/ml, titania nanotube and bromo Dopamine hydrochloride is 0.5:1-2:1；
(4) the bromo titania nanotube in step (3) is dissolved in solvent and forms solution, by going back in step (2)
Raw cotton fabric is immersed in solution, adds triethylamine, is stirred, and is dried, is obtained titania nanotube/cotton based on click chemistry and knit
Object light catalysis material, wherein reduction bafta, bromo titania nanotube, solvent, the ratio of triethylamine are (0.5-2g):
(1.0-3.0g):(30-50ml):(0.2-1ml)。
The specific steps for pre-processing bafta in the step (1)：By sodium hydroxide and paregal O using mass ratio as 1:
1-1:4 formation mixed solutions soluble in water, bafta is placed in mixed solution, ultrasonic 10- under the conditions of being 50-80 DEG C in temperature
30min, obtain pre-processing bafta, the wherein mass ratio of bafta and sodium hydroxide is 1:1-4:1, hydroxide in mixed solution
The concentration of sodium is 3-8g/l.
Reducing agent is silane coupler in the step (2)；Solvent is that volume ratio is 4:1 second alcohol and water.
The pH value of reductant solution is 3-4 in the step (2), is adjusted with the boric acid solution that pH value is 2.0.
Mixing time is 0.5-1h in the step (2), and whipping temp is 20-30 DEG C；The immersion time is 1-5min.
Drying is carried out in vacuum drying oven in the step (2), drying time 5-10min, drying temperature 100-
130℃。
The preparation method of bromo Dopamine hydrochloride is in the step (3)：Ten water Boratexes are dissolved in water, in N2Under environment
Add Dopamine hydrochloride and form mixed solution, stir 10-30min, 2- is added dropwise under the conditions of temperature is -5-0 DEG C of ice-water baths
Bromine isobutyl acylbromide, time 20-40min, N2Continue to stir 18-24h under environment, pH value is 9-10 in course of reaction, adds salt
Acid solution, extract, dry, separation, bromo Dopamine hydrochloride is obtained, wherein the concentration of ten water dobell's solutions is 0.01-
The mass ratio of 0.075g/ml, ten water Boratexes and Dopamine hydrochloride is 1:1-4:1, ten water Boratexes and 2- bromine isobutyl acylbromides
Than for 2g:1.5ml-6g:1.0ml.
The pH value of the mixed solution is 9-10；The concentration of hydrochloric acid solution is 5-8mol/l.
The extraction extracts for ethyl acetate, and extraction times is three times；Dry and be for anhydrous magnesium sulfate drying, drying time
12-15h。
Solvent is that volume ratio is 2 in the step (3):1-8:1 ethanol and deionized water；Ultrasonic time is 1-2h.
Step (3) the lucifuge mixing time is 2-4h；It is 15-20h that lucifuge, which continues mixing time,.
Washing is to be washed successively with deionized water and ethanol in the step (3).
Step (3) drying is carried out in vacuum drying oven, drying time 20-30h, and drying temperature is 40-60 DEG C.
Solvent is that volume ratio is 1 in the step (4):1 second alcohol and water.
The time of stirring is 1-2h in the step (4), and the temperature of stirring is 20-30 DEG C.
Drying is carried out in vacuum drying oven in the step (4), and drying temperature is 40-60 DEG C.
The titania nanotube based on click chemistry/bafta catalysis material is used to adsorb and printed in the step (4)
Contaminate the dyestuff in waste water.
A kind of preparation method of the titania nanotube based on click chemistry/bafta catalysis material of the present invention,
Thiol group is produced first by silane coupler on the surface of pretreatment bafta as reducing agent to obtain reducing bafta, so
Bromo Dopamine hydrochloride is grafted to titania nanotube surface by the way of dehydrating condensation afterwards and obtains bromo titanium dioxide
Nanotube, finally bromo titania nanotube and reduction bafta are formed with mercaptan-halogen using the method for click chemistry
Covalent bond, bromo titania nanotube is set to be supported on the surface of reduction bafta.
Beneficial effect
(1) method of the invention is simple, and cost is low, and mild condition, product yield high, side reaction is few, environmental protection；
(2) titania nanotube based on click chemistry that the present invention is prepared/bafta catalysis material absorption
Efficiency high, stability is good, has good photocatalysis effect and the excellent feature of environmental protection, can be used for the place of dyestuff in dyeing waste water
Reason, application of the bafta in terms of waste water from dyestuff is adsorbed in photocatalysis is widened, has breached conventional coatings carried titanium dioxide nanometer
The deficiency of kind fabric is adsorbed in pipe photocatalysis, is overcome the nano-titanium dioxide powder material in the presence of prior art and is easily reunited
And reclaim the problem of difficult.
Brief description of the drawings
Fig. 1 is the process chart of bromo titania nanotube in the present invention；
Fig. 2 is the process chart that bafta is reduced in the present invention；
Fig. 3 is the work that the bromo titania nanotube synthesized in the present invention is reacted with reduction bafta by click chemistry
Skill flow chart；
Fig. 4 is to test the titanium dioxide based on click chemistry in (a) embodiment 1 using ultraviolet specrophotometer in embodiment 5
The adsorption effect figure of titanium nanotube/bafta catalysis material and (b) titania nanotube.
Embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate the present invention
Rather than limitation the scope of the present invention.In addition, it is to be understood that after the content of the invention lectured has been read, people in the art
Member can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited
Scope.
In the embodiment of the present invention, the bafta used is purchased from Chinese Saintyear Holding Group Co., Ltd., and silane used is even
Connection agent is purchased from this reagent Co., Ltd of Dutch Hadamard, and titania nanotube used works perseveringly nano material purchased from Guangdong Huizhou
Co., Ltd, 2- bromine isobutyl acylbromides (98%) used are purchased from Beijing Yi Nuokai Science and Technology Ltd.s.Used in experiment other
Chemicals is purchased from traditional Chinese medicines chemical reagent Co., Ltd.All reagents are that analysis is pure, in use without further carrying
It is pure.
Embodiment 1
(1) 0.5g sodium hydroxides and 0.7g paregal Os are dissolved in 100ml water and form mixed solution, by 1g baftas
(6cm × 6cm) is placed in mixed solution, and ultrasonic wave cleans 20min under 70 DEG C of water bath conditions, removes the greasy dirt of fabric face, obtains
To pretreatment bafta.
(2) 2g silane couplers are dissolved in 50ml volume ratios for 4:Solution is formed in 1 second alcohol and water, is 2.0 with pH value
Boric acid solution regulation solution pH value to 3-4,30min is stirred under the conditions of 25 DEG C, by the pretreatment bafta in step (1)
0.98g immerses 2min in the solution, is placed in 120 DEG C of vacuum drying ovens and dries 5min, obtains reducing bafta.
(3) the water Boratexes of 4g ten are added in 250mL three-neck flasks and 100ml water forms solution, use N2Purge 30min,
1.9g Dopamine hydrochlorides are added, 15min is stirred by 100 rpms of speed, and it is 9-10 to adjust reaction solution pH, by gained
Solution cooled down in 0 DEG C of ice-water bath, 1.2ml 2- bromine isobutyl acylbromides are added dropwise into bottle in 30min, in N2100 under environment
Rpm speed continue to stir 24h, course of reaction keeps pH to maintain 9-10, and after reaction terminates, addition concentration is 6mol/
The pH value of l hydrochloric acid solution regulation solution is 2, with the extraction of 100ml ethyl acetate three times, merges organic phase, adds anhydrous MgSO4
12h is dried, rotary evaporation removes ethyl acetate afterwards, obtains brown viscous liquid, and column chromatography is carried out to viscous brown crude product
Separation, by the use of methanol and chloroform mixed solution as solvent, the wherein percentage by volume of methanol is 5%, obtains bromo
Dopamine hydrochloride.
(4) 50mg titania nanotubes are weighed in 100mL single-necked flasks, add 8ml deionized waters and 32ml ethanol,
Ultrasonic 1h, normal temperature lucifuge stir 3h by 100 rpms of speed, the bromo Dopamine hydrochloride 40mg added in step (3),
Continue stirring 18h by 100 rpms of speed under normal temperature lucifuge, then clean deionized water repeatedly with deionized water and ethanol
Gained precipitates, and dries 24h with 50 DEG C of vacuum drying ovens, obtains bromo titania nanotube.
(5) the bromo titania nanotube in 1g steps (4) is dissolved in 30ml volume ratios for 1:Shape in 1 second alcohol and water
Into solution, the reduction bafta 0.95g in step (2) is immersed in solution, addition 0.3ml triethylamines, under 30 DEG C of water bath conditions
Heating stirring 1h, it is placed in 50 DEG C of vacuum drying ovens and dries, obtains the titania nanotube based on click chemistry/bafta light and urge
Change material.
Embodiment 2
(1) 0.5g sodium hydroxides and 0.7g paregal Os are dissolved in 100ml water and form mixed solution, by 1g baftas
(6cm × 6cm) is placed in mixed solution, and ultrasonic wave cleans 20min under 70 DEG C of water bath conditions, removes the greasy dirt of fabric face, obtains
To pretreatment bafta.
(2) 2g silane couplers are dissolved in 50ml volume ratios for 4:Solution is formed in 1 second alcohol and water, is 2.0 with pH value
Boric acid solution regulation solution pH value to 3-4,30min is stirred under the conditions of 25 DEG C, by the pretreatment bafta in step (1)
0.98g immerses 2min in the solution, is placed in 120 DEG C of vacuum drying ovens and dries 5min, obtains reducing bafta.
(3) the water Boratexes of 4g ten are added in 250mL three-neck flasks and 100ml water forms solution, use N2Purge 30min,
1.9g Dopamine hydrochlorides are added, 15min is stirred by 100 rpms of speed, and it is 9-10 to adjust reaction solution pH, by gained
Solution cooled down in 0 DEG C of ice-water bath, 1.2ml 2- bromine isobutyl acylbromides are added dropwise into bottle in 30min, in N2100 under environment
Rpm speed continue to stir 24h, course of reaction keeps pH to maintain 9-10, and after reaction terminates, addition concentration is 6mol/
The pH value of l hydrochloric acid solution regulation solution is 2, with the extraction of 100ml ethyl acetate three times, merges organic phase, adds anhydrous MgSO4
12h is dried, rotary evaporation removes ethyl acetate afterwards, obtains brown viscous liquid, and column chromatography is carried out to viscous brown crude product
Separation, by the use of methanol and chloroform mixed solution as solvent, the wherein percentage by volume of methanol is 5%, obtains bromo
Dopamine hydrochloride.
(4) 100mg titania nanotubes are weighed in 100mL single-necked flasks, add 16ml deionized waters and 64ml second
Alcohol, ultrasonic 1h, normal temperature lucifuge is by 100 rpms of speed stirring 3h, the bromo Dopamine hydrochloride added in step (3)
80mg, continue stirring 18h by 100 rpms of speed under normal temperature lucifuge, then cleaned repeatedly with deionized water and ethanol
Precipitated obtained by deionized water, dry 24h with 50 DEG C of vacuum drying ovens, obtain bromo titania nanotube.
(5) the bromo titania nanotube in 2g steps (4) is dissolved in 50ml volume ratios for 1:Shape in 1 second alcohol and water
Into solution, the reduction bafta 0.95g in step (2) is immersed in solution, addition 0.5ml triethylamines, under 30 DEG C of water bath conditions
Heating stirring 1h, it is placed in 50 DEG C of vacuum drying ovens and dries, obtains the titania nanotube based on click chemistry/bafta light and urge
Change material.
Embodiment 3
(1) 0.5g sodium hydroxides and 0.7g paregal Os are dissolved in 100ml water and form mixed solution, by 1g baftas
(6cm × 6cm) is placed in mixed solution, and ultrasonic wave cleans 20min under 70 DEG C of water bath conditions, removes the greasy dirt of fabric face, obtains
To pretreatment bafta.
(2) 1.25g silane couplers are dissolved in 30ml volume ratios for 4:Solution is formed in 1 second alcohol and water, is with pH value
The pH value of 2.0 boric acid solution regulation solution stirs 30min, by the pretreatment cotton in step (1) to 3-4 under the conditions of 25 DEG C
Fabric 0.98g immerses 4min in the solution, is placed in 120 DEG C of vacuum drying ovens and dries 5min, obtains reducing bafta.
(3) the water Boratexes of 4g ten are added in 250mL three-neck flasks and 100ml water forms solution, use N2Purge 30min,
1.9g Dopamine hydrochlorides are added, 15min is stirred by 100 rpms of speed, and it is 9-10 to adjust reaction solution pH, by gained
Solution cooled down in 0 DEG C of ice-water bath, 1.2ml 2- bromine isobutyl acylbromides are added dropwise into bottle in 30min, in N2100 under environment
Rpm speed continue to stir 24h, course of reaction keeps pH to maintain 9-10, and after reaction terminates, addition concentration is 6mol/
The pH value of l hydrochloric acid solution regulation solution is 2, with the extraction of 100ml ethyl acetate three times, merges organic phase, adds anhydrous MgSO4
12h is dried, rotary evaporation removes ethyl acetate afterwards, obtains brown viscous liquid, and column chromatography is carried out to viscous brown crude product
Separation, by the use of methanol and chloroform mixed solution as solvent, the wherein percentage by volume of methanol is 5%, obtains bromo
Dopamine hydrochloride.
(4) 50mg titania nanotubes are weighed in 100mL single-necked flasks, add 8ml deionized waters and 32ml ethanol,
Ultrasonic 1h, normal temperature lucifuge stir 3h by 100 rpms of speed, the bromo Dopamine hydrochloride 40mg added in step (3),
Continue stirring 18h by 100 rpms of speed under normal temperature lucifuge, then clean deionized water repeatedly with deionized water and ethanol
Gained precipitates, and dries 24h with 50 DEG C of vacuum drying ovens, obtains bromo titania nanotube.
(5) the bromo titania nanotube in 1g steps (4) is dissolved in 30ml volume ratios for 1:Shape in 1 second alcohol and water
Into solution, the reduction bafta 0.96g in step (2) is immersed in solution, addition 0.3ml triethylamines, under 30 DEG C of water bath conditions
Heating stirring 1h, it is placed in 50 DEG C of vacuum drying ovens and dries, obtains the titania nanotube based on click chemistry/bafta light and urge
Change material.
Embodiment 4
(1) 0.5g sodium hydroxides and 0.7g paregal Os are dissolved in 100ml water and form mixed solution, by 1g baftas
(6cm × 6cm) is placed in mixed solution, and ultrasonic wave cleans 20min under 70 DEG C of water bath conditions, removes the greasy dirt of fabric face, obtains
To pretreatment bafta.
(2) 2g silane couplers are dissolved in 50ml volume ratios for 4:Solution is formed in 1 second alcohol and water, is 2.0 with pH value
Boric acid solution regulation solution pH value to 3-4,30min is stirred under the conditions of 25 DEG C, by the pretreatment bafta in step (1)
0.98g immerses 2min in the solution, is placed in 120 DEG C of vacuum drying ovens and dries 5min, obtains reducing bafta.
(3) the water Boratexes of 4g ten are added in 250mL three-neck flasks and 100ml water forms solution, use N2Purge 30min,
1.9g Dopamine hydrochlorides are added, 15min is stirred by 100 rpms of speed, and it is 9-10 to adjust reaction solution pH, by gained
Solution cooled down in 0 DEG C of ice-water bath, 1.2ml 2- bromine isobutyl acylbromides are added dropwise into bottle in 30min, in N2100 under environment
Rpm speed continue to stir 24h, course of reaction keeps pH to maintain 9-10, and after reaction terminates, addition concentration is 6mol/
The pH value of l hydrochloric acid solution regulation solution is 2, with the extraction of 100ml ethyl acetate three times, merges organic phase, adds anhydrous MgSO4
12h is dried, rotary evaporation removes ethyl acetate afterwards, obtains brown viscous liquid, and column chromatography is carried out to viscous brown crude product
Separation, by the use of methanol and chloroform mixed solution as solvent, the wherein percentage by volume of methanol is 5%, obtains bromo
Dopamine hydrochloride.
(4) 50mg titania nanotubes are weighed in 100mL single-necked flasks, add 8ml deionized waters and 32ml ethanol,
Ultrasonic 1h, normal temperature lucifuge stir 3h by 100 rpms of speed, the bromo Dopamine hydrochloride 40mg added in step (3),
Continue stirring 18h by 100 rpms of speed under normal temperature lucifuge, then clean deionized water repeatedly with deionized water and ethanol
Gained precipitates, and dries 24h with 50 DEG C of vacuum drying ovens, obtains bromo titania nanotube.
(5) the bromo titania nanotube in 1g steps (4) is dissolved in 50ml volume ratios for 1:Shape in 1 second alcohol and water
Into solution, the reduction bafta 0.95g in step (2) is immersed in solution, addition 0.5ml triethylamines, under 30 DEG C of water bath conditions
Heating stirring 1h, it is placed in 50 DEG C of vacuum drying ovens and dries, obtains the titania nanotube based on click chemistry/bafta light and urge
Change material.
Embodiment 5
Using the titania nanotube based on click chemistry prepared in ultraviolet specrophotometer testing example 1/
The absorbance of dyestuff in the front and rear absorption dyeing waste water of bafta catalysis material illumination.By in embodiment 1 based on click chemistry
Titania nanotube/bafta catalysis material and titania nanotube are respectively placed in the dyestuff configured, reaction
10min, while its rate of adsorption is observed, and absorbance is measured, 60min is then reacted under ultraviolet irradiation condition and observes it simultaneously
The rate of adsorption, and measure absorbance (see Fig. 4).As a result show that the titania nanotube based on click chemistry/bafta light is urged
It is high to change material adsorption efficiency, stability is good, has good photocatalysis effect and the excellent feature of environmental protection.
Claims (10)
1. a kind of preparation method of the titania nanotube based on click chemistry/bafta catalysis material, specific steps are such as
Under:
(1) bafta is pre-processed, obtains pre-processing bafta；
(2) dissolve reduce agent in and reductant solution is formed in solvent, stir, the pretreatment bafta in step (1) is immersed also
In former agent solution, dry, obtain reducing bafta, the wherein concentration of reductant solution be 0.01-0.05g/ml, reducing agent with advance
The ratio for handling bafta is 1:1-3:1；
(3) titania nanotube is dissolved in solvent and forms solution, ultrasound, lucifuge stirring, added bromo Dopamine hydrochloride, keep away
Light continues to stir, and washs, and dries, obtains bromo titania nanotube, wherein titania nanotube solution concentration is 0.6-
The mass ratio of 2.4mg/ml, titania nanotube and bromo Dopamine hydrochloride is 0.5:1-2:1；
(4) the bromo titania nanotube in step (3) is dissolved in solvent and forms solution, raw cotton will be gone back in step (2)
Fabric is immersed in solution, adds triethylamine, is stirred, and is dried, is obtained the titania nanotube based on click chemistry/bafta light
Catalysis material, wherein reduction bafta, bromo titania nanotube, solvent, the ratio of triethylamine are (0.5-2g):(1.0-
3.0g):(30-50ml):(0.2-1ml)。
2. according to a kind of titania nanotube based on click chemistry/bafta catalysis material described in claim 1
Preparation method, it is characterised in that the specific steps for pre-processing bafta in the step (1)：By sodium hydroxide and paregal O
Using mass ratio as 1:1-1:4 formation mixed solutions soluble in water, bafta is placed in mixed solution, is 50-80 DEG C in temperature
Under the conditions of ultrasonic 10-30min, obtain pre-process bafta, wherein the mass ratio of bafta and sodium hydroxide be 1:1-4:1, mix
The concentration for closing sodium hydroxide in solution is 3-8g/l.
3. according to a kind of titania nanotube based on click chemistry/bafta catalysis material described in claim 1
Preparation method, it is characterised in that reducing agent is silane coupler in the step (2)；Solvent is that volume ratio is 4:1 ethanol and
Water；The pH value of reductant solution is 3-4, is adjusted with the boric acid solution that pH value is 2.0.
4. according to a kind of titania nanotube based on click chemistry/bafta catalysis material described in claim 1
Preparation method, it is characterised in that mixing time is 0.5-1h in the step (2), and whipping temp is 20-30 DEG C；Immerse the time
For 1-5min；Drying is carried out in vacuum drying oven, drying time 5-10min, and drying temperature is 100-130 DEG C.
5. according to a kind of titania nanotube based on click chemistry/bafta catalysis material described in claim 1
Preparation method, it is characterised in that the preparation method of bromo Dopamine hydrochloride is in the step (3)：Ten water Boratexes are dissolved in
Water, in N2Dopamine hydrochloride is added under environment and forms mixed solution, 10-30min is stirred, is -5-0 DEG C of ice-water bath conditions in temperature
Under 2- bromine isobutyl acylbromides, time 20-40min, N is added dropwise2Continue to stir 18-24h under environment, pH value is in course of reaction
9-10, hydrochloric acid solution is added, extracted, dried, separation, bromo Dopamine hydrochloride is obtained, wherein the concentration of ten water dobell's solutions
For 0.01-0.075g/ml, the mass ratio of ten water Boratexes and Dopamine hydrochloride is 1:1-4:1, ten water Boratexes and 2- bromine isobutyls
The ratio of acylbromide is 2g:1.5ml-6g:1.0ml.
6. according to a kind of titania nanotube based on click chemistry/bafta catalysis material described in claim 5
Preparation method, it is characterised in that the pH value of the mixed solution is 9-10；The concentration of hydrochloric acid solution is 5-8mol/l；Extract and be
Ethyl acetate extracts, and extraction times is three times；Dry and dried for anhydrous magnesium sulfate, drying time 12-15h.
7. according to a kind of titania nanotube based on click chemistry/bafta catalysis material described in claim 1
Preparation method, it is characterised in that solvent is that volume ratio is 2 in the step (3):1-8:1 ethanol and deionized water；When ultrasonic
Between be 1-2h；Lucifuge mixing time is 2-4h；It is 15-20h that lucifuge, which continues mixing time,.
8. according to a kind of titania nanotube based on click chemistry/bafta catalysis material described in claim 1
Preparation method, it is characterised in that washing is to be washed successively with deionized water and ethanol in the step (3)；Drying is in vacuum
Carried out in baking oven, drying time 20-30h, drying temperature is 40-60 DEG C.
9. according to a kind of titania nanotube based on click chemistry/bafta catalysis material described in claim 1
Preparation method, it is characterised in that solvent is that volume ratio is 1 in the step (4):1 second alcohol and water；The time of stirring is 1-
2h, the temperature of stirring is 20-30 DEG C；Drying is carried out in vacuum drying oven, and drying temperature is 40-60 DEG C.
10. according to a kind of titania nanotube based on click chemistry/bafta catalysis material described in claim 1
Preparation method, it is characterised in that the titania nanotube based on click chemistry/bafta photocatalysis material in the step (4)
Expect for adsorbing the dyestuff in dyeing waste water.
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| CN111926562A (en) * | 2020-07-08 | 2020-11-13 | 武汉纺织大学 | ZIF-8 composite TiO2Functional fabric and preparation method thereof |
| CN112661969A (en) * | 2020-12-02 | 2021-04-16 | 张茜茜 | Antibacterial echinoid TiO2Grafted polyethylene film material and preparation method thereof |
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