CN109908886A - The preparation method and product of a kind of doping stannic oxide hydrosol and its application in cotton fabric automatically cleaning - Google Patents
The preparation method and product of a kind of doping stannic oxide hydrosol and its application in cotton fabric automatically cleaning Download PDFInfo
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- CN109908886A CN109908886A CN201910263737.5A CN201910263737A CN109908886A CN 109908886 A CN109908886 A CN 109908886A CN 201910263737 A CN201910263737 A CN 201910263737A CN 109908886 A CN109908886 A CN 109908886A
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Abstract
The invention discloses a kind of preparation method of doping stannic oxide hydrosol and product and its applications in cotton fabric automatically cleaning, including, weigh glass putty and stannic chloride pentahydrate, distilled water dissolution is added, it is added to after stirring in the stainless steel cauldron with polytetrafluoroethyllining lining, it is baked for 24 hours in 180 DEG C of high temperature of baking oven, cooling 5h removes supernatant liquor, and lower sediment is placed in centrifuge tube, after 10000rpm is centrifuged 5min, taking precipitate is washed 1 time, dehydrated alcohol is added to wash 3 times, is centrifuged 5min, takes to be deposited in baking oven and dry, grinding, obtains doping stannic oxide crystal；Weigh the 3 of 8mg, 4- dihydroxyphenyl acetic acid is dissolved into 50mL distilled water, is ultrasonically treated 5min, magnetic stirrer 10min, 0.5g doping stannic oxide crystal is added, stirs 10min, obtains the doping stannic oxide hydrosol, for finishing of cotton textiles, while providing cotton fabric significant self-cleaning performance, nanoparticle and fabric binding force can be improved, improves fastness.
Description
Technical field
The present invention relates to cotton fabric automatically cleaning fields, more particularly to a kind of preparation method of doping stannic oxide hydrosol
With product and its application in cotton fabric automatically cleaning.
Background technique
Stannic oxide is a kind of semiconductor that band-gap energy is 3.6eV, is insulated under room temperature, crystalline silica tin is tetragonal
The square crystal of system, structure is simple, at low cost, long service life.Stannic oxide is usually used in various micro low volume fraction gas
The detection of body, in Sensitive Apparatus, glass electrode, ceramics, the extensive use of the methods of solar battery.Pure tin dioxide photocatalyst
Due to forbidden bandwidth about 3.5eV, it is seen that photolytic activity is poor, and photo-generate electron-hole is easily compound, to improve photocatalysis performance, often
Realized using the method for doping, a kind of effective method be by doped metallic elements or nonmetalloid, doping with
Afterwards, the enhancing of separation photo-generated carrier ability, light induced electron and hole-recombination ability reduce, and photocatalysis efficiency is improved, can be with
Accelerate the degradation of organic pollutant.Traditional element doping will lead to the calorifics unstability of semiconductor, while also increase electricity
Son-hole is to again compound reaction center.
The frequent washing of textile can allow it to lose its original color and shape, can also make the fibre damage of fabric, and
When other textiles clean together, also other textiles can be made to be stain by it, often washing can waste water resource.Pass through photocatalysis
Automatically cleaning technology, nano-photocatalyst pass through oxidation and reduction degradation surface attachment or absorption under solar radiation
Organic matter, inorganic matter or microorganism.
In recent years, textile uses nano-titanium dioxide as catalysis material more, and titanium dioxide property is stablized, nontoxic,
Small with particle, the characteristics of thermal conductance is good, large specific surface area, good dispersion, photocatalytic activity is stablized, and photoelectric conversion ability
It is good, but titanium dioxide is not easy to disperse in apolar substance, and easy aggregation and organic solvent are affine in polar substances
The poor and fabric of property is not easy to combine.
Summary of the invention
The purpose of this section is to summarize some aspects of the embodiment of the present invention and briefly introduce some preferable implementations
Example.It may do a little simplified or be omitted to avoid our department is made in this section and the description of the application and the title of the invention
Point, the purpose of abstract of description and denomination of invention it is fuzzy, and this simplification or omit and cannot be used for limiting the scope of the invention.
In view of the above-mentioned and/or existing doping stannic oxide hydrosol preparation method the problem of, propose this hair
It is bright.
Therefore, the one of purpose of the present invention is to overcome the shortcomings of the preparation method of the existing doping stannic oxide hydrosol,
A kind of preparation method of doping stannic oxide hydrosol is provided, including, it prepares doping stannic oxide crystal: weighing suitable glass putty
And stannic chloride pentahydrate, distilled water dissolution is added, is added to after stirring in the stainless steel cauldron with polytetrafluoroethyllining lining, in
180 DEG C of high temperature of baking oven bake for 24 hours, after cooling 5h, remove supernatant liquor, and lower sediment is placed in centrifuge tube, 10000rpm centrifugation
After 5min, taking precipitate is washed 1 time, and dehydrated alcohol is added, and to washing of precipitate 3 times, after 10000rpm is centrifuged 5min, takes precipitating
It is dried in baking oven, grinds, obtain doping stannic oxide crystal；The preparation auto-dope stannic oxide hydrosol: the 3,4- bis- of 8mg is weighed
Hydroxyphenyl acetic acid is dissolved into 50mL distilled water, is ultrasonically treated 5min, magnetic stirrer 10min, is added described in 0.5g
Doping stannic oxide crystal stirs 10min to get the auto-dope stannic oxide hydrosol.
A kind of preferred embodiment of preparation method as the doping stannic oxide hydrosol of the present invention, in which: the system
Standby doping stannic oxide crystal, wherein the molar ratio of glass putty and stannic chloride pentahydrate is 3:2~3.
A kind of preferred embodiment of preparation method as the doping stannic oxide hydrosol of the present invention, in which: the tin
The molar ratio of powder and stannic chloride pentahydrate is 3:2.
A kind of preferred embodiment of preparation method as the doping stannic oxide hydrosol of the present invention, in which: described to take
It is deposited in baking oven and dries, wherein oven temperature is 60 DEG C, and the drying and processing time is 30min.
A kind of preferred embodiment of preparation method as the doping stannic oxide hydrosol of the present invention, in which: the system
The standby auto-dope stannic oxide hydrosol, wherein sonification power 50KHz, treatment temperature are 30 DEG C.
A kind of preferred embodiment of preparation method as the doping stannic oxide hydrosol of the present invention, in which: the magnetic
Power blender stirs 10min, wherein speed of agitator 700rpm.
A kind of preferred embodiment of preparation method as the doping stannic oxide hydrosol of the present invention, in which: described to add
Enter doping stannic oxide crystal described in 0.5g, stir 10min to get the auto-dope stannic oxide hydrosol, wherein stirs and be
Mechanical stirring, speed of agitator 800rpm.
Another object of the present invention is to provide a kind of preparation method doping two obtained of auto-dope stannic oxide hydrosol
The tin oxide hydrosol.
Further object of the present invention is to provide a kind of auto-dope stannic oxide hydrosol answering in cotton fabric automatically cleaning
With.
Advantageous effects of the present invention:
(1) present invention provides a kind of preparation method of auto-dope stannic oxide hydrosol, with glass putty and tin tetrachloride according to
Certain ratio Direct Hydrothermal reaction prepares the stannic oxide crystal of Lacking oxygen, and surface has a large amount of hydroxyl, adulterates two with this
Tin oxide crystal prepares the auto-dope stannic oxide hydrosol, is applied in cotton fabric automatically cleaning, can reinforce colloidal sol and cotton fabric is fine
The binding force of dimension.
(2) present invention provides a kind of preparation method of auto-dope stannic oxide hydrosol, with glass putty and tin tetrachloride according to
Certain ratio Direct Hydrothermal reaction prepares the stannic oxide crystal of Lacking oxygen, is modified with 3,4- dihydroxyphenyl acetic acid, improves
The stability of colloidal sol, cotton fabric carry out cation-modified, increase the electrostatic attraction of the stannic oxide hydrosol and fabric, raising is received
Rice corpuscles and fabric binding force improve fastness.
(3) a kind of auto-dope stannic oxide hydrosol has been made in the present invention, is used for finishing of cotton textiles, and providing cotton fabric is significant
Self-cleaning performance while, can improve nanoparticle and fabric binding force, improve fastness.
Detailed description of the invention
In order to illustrate the technical solution of the embodiments of the present invention more clearly, required use in being described below to embodiment
Attached drawing be briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for this
For the those of ordinary skill of field, without any creative labor, it can also be obtained according to these attached drawings other
Attached drawing.Wherein:
Fig. 1 is the XRD diagram that auto-dope stannic oxide is made in the embodiment of the present invention 1.
Fig. 2 is the transmission electron microscope picture that auto-dope stannic oxide is made in the embodiment of the present invention 1.
Fig. 3 is the infrared spectroscopy of auto-dope stannic oxide made from the embodiment of the present invention 1.
Fig. 4 is auto-dope stannic oxide photoelectricity flow graph made from the embodiment of the present invention 1.
Fig. 5 is the molar ratio of difference of embodiment of the present invention glass putty and tin tetrachloride to photocatalytic degradation curve.
Fig. 6 is cotton fabric SEM figure in the embodiment of the present invention.
Fig. 7 is the Fourier Transform Infrared Spectroscopy figure of cotton fabric during the present invention is implemented.
Fig. 8 is that finishing of cotton textiles and raw cotton fabric are bent to the Visible Light Induced Photocatalytic dynamics of methylene blue in the embodiment of the present invention
Line chart.
Fig. 9 is the colour fading figure being added dropwise in finishing of cotton textiles after red wine under visible optical radiation in the embodiment of the present invention.
Figure 10 is that different cotton fabric processing modes are bent to the Visible Light Induced Photocatalytic dynamics of methylene blue in the embodiment of the present invention
Line chart.
Specific embodiment
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, below with reference to specification embodiment
Specific embodiments of the present invention will be described in detail.
In the following description, numerous specific details are set forth in order to facilitate a full understanding of the present invention, but the present invention can be with
Implemented using other than the one described here other way, those skilled in the art can be without prejudice to intension of the present invention
In the case of do similar popularization, therefore the present invention is not limited by the specific embodiments disclosed below.
Secondly, " one embodiment " or " embodiment " referred to herein, which refers to, may be included at least one realization side of the invention
A particular feature, structure, or characteristic in formula." in one embodiment " that different places occur in the present specification not refers both to
The same embodiment, nor the individual or selective embodiment mutually exclusive with other embodiments.
Embodiment 1
It prepares doping stannic oxide crystal: weighing suitable glass putty 0.36g (0.003mol) and stannic chloride pentahydrate 0.7g
(0.002mol) is added 60mL distilled water, is added in the stainless steel cauldron with polytetrafluoroethyllining lining after stirring, in baking oven
180 DEG C of high temperature bake for 24 hours, after cooling 5h, remove supernatant liquor, and lower sediment is placed in centrifuge tube, and 10000rpm is centrifuged 5min,
8mL distilled water is added in taking precipitate, washes 1 time, and 8mL ethyl alcohol is added, after carrying out washing 3 times to precipitating, 10000rpm centrifugation
Precipitating is placed in 60 DEG C of baking oven and dries 30min by 5min, is placed in grinding in the container of grinding, obtains the doping stannic oxide
Crystal；
It prepares the doping stannic oxide hydrosol: weighing 3, the 4- dihydroxyphenyl acetic acid of 8mg, be dissolved into 50mL distilled water
In, 10min is stirred under the conditions of 50KHz, 30 DEG C of ultrasonic treatments 5min, magnetic stirring apparatus 700rpm, and 0.5g is added and adulterates titanium dioxide
Tin crystal, 800rpm stir 10min to get the auto-dope stannic oxide hydrosol.
X-ray diffraction test has been carried out to stannic oxide and auto-dope stannic oxide, has seen Fig. 1.It mixes certainly as can be seen from Figure 1
Miscellaneous stannic oxide does not have the peak of other impurities, illustrates that the catalyst purity of the method preparation is very high, SnO2Main diffraction peak exist
At 26.50 °, 32.98 °, 37.59 °, 52.10 °, 66.08 ° and 77.91 °, (110) (101) of Rutile Type are respectively corresponded
(200)(211)(301).By Scherrer formula, by calculating, grain size is about 4.6nm.Auto-dope stannic oxide with do not mix
The crystal form of miscellaneous stannic oxide is consistent, crystallization position of the divalent tin ion instead of tetravalence tin ion.The storage of auto-dope stannic oxide
It is good to deposit stability, after storage 3 months, catalytic activity is not reduced.
The transmission electron microscope picture of auto-dope stannic oxide is shown in Fig. 2, and as shown in Figure 2, auto-dope stannic oxide is irregular
Grain, dispersion performance is poor in ethanol solution, and this point also has embodiment during washing from centrifugation ethyl alcohol.By calculating, particle is big
It is about 4.5 nanometers small, it is consistent with XRD test result.It may know that by high power projection electron microscope, interplanar distance is that 0.33nm corresponds to golden red
Stannic oxide (110) crystal face of stone phase, it is also consistent with XRD test result.Light-catalyzed reaction is surface reaction, the grain of photochemical catalyst
Diameter is small, large specific surface area, shows that the active point of reaction is more, photocatalysis performance improves.
Fig. 3 is the infrared spectrogram of auto-dope stannic oxide obtained, is (a) infrared spectrogram before modified in figure, (b) changes
Infrared spectrogram after property, it can be seen that wavelength is near 3424 and 1632, and the peak of appearance is it is obvious that these peaks demonstrate cotton
The presence of upper hydroxyl, the peak at 1632 is bending vibration, and the peak at 3424 is stretching vibration, and comparison is found afterwards before modified, modified
More a peak, this peak prove that modifying agent is successfully modified on catalyst at 1258 afterwards, the presence at these peaks, it was demonstrated that hydroxyl-
Crosslinking is possible between hydroxyl.
Fig. 4 is the photoelectricity flow graph of auto-dope stannic oxide obtained, is (a) SnO in figure2- x photoelectricity flow graph (b) is SnO2
Photoelectricity flow graph.From this figure as can be seen that in illumination, current density becomes larger, and electric current becomes smaller when being protected from light, auto-dope SnO2-x light
Electric current is approximately SnO2Two times, and repeat to test several times, conclusion is essentially identical, illustrates both different photochemical catalysts examinations
The density of photocurrent of sample is more stable.And photoelectric current is high, illustrates that the separative efficiency of photo-generate electron-hole is high, the utilization rate of photon
It is high.The photocatalysis performance of auto-dope stannic oxide will be better than stannic oxide.
Embodiment 2
It prepares doping stannic oxide crystal: weighing suitable glass putty 0.36g (0.003mol) and stannic chloride pentahydrate 0.7g
(0.002mol) is added 60mL distilled water, is added in the stainless steel cauldron with polytetrafluoroethyllining lining after stirring, in baking oven
180 DEG C of high temperature bake for 24 hours, after cooling 5h, remove supernatant liquor, and lower sediment is placed in centrifuge tube, and 10000rpm is centrifuged 5min,
8mL distilled water is added in taking precipitate, washes 1 time, and 8mL ethyl alcohol is added, after carrying out washing 3 times to precipitating, 10000rpm centrifugation
Precipitating is placed in 60 DEG C of baking oven and dries 30min by 5min, is placed in grinding in the container of grinding, obtains the doping stannic oxide
Crystal.
In order to find preferable catalyst formulation, the glass putty and tin tetrachloride of different mol ratio are had studied, its light is measured and urges
Change activity, sees Fig. 5.It can be seen from the figure that most preferably molar ratio is 3:2 to degradation rate in same time.With Theil indices
Increase, light degradation property improves.Disproportionated reaction occurs for tin and tin tetrachloride, generates Bivalent Tin, and stannous content increases, it is seen that
Photolytic activity increases.Since divalent tin dope is to enter lattice, do not find that miscellaneous peak also determines this point from XRD diagram.It is stannous
It is entrained between the conduction band of stannic oxide and valence band and forms Lacking oxygen.Under visible optical radiation, stannic oxide since forbidden bandwidth is big,
Electronics in valence band is difficult to be energized on conduction band.Due to there is the presence of the defects of Lacking oxygen state in auto-dope stannic oxide forbidden band,
Under the conditions of visible optical radiation, the electronics in valence band can be transitted on Lacking oxygen, then under the lower light radiation of energy, jump
It adjourns on the conduction band of stannic oxide, participates in light-catalyzed reaction.Bivalent Tin can capture hole, be conducive to light induced electron and hole
Separation so photocatalytic activity improves with the increase of divalent Theil indices, but as the dosage of glass putty increases, adulterates Bivalent Tin
Content increase, increase to a certain extent after, will become electron-hole complex centre, so that Photocatalytic Degradation Property is reduced.
Photocatalytic activity test: light source is PLS-SXE type 300W steady current source for xenon lamp, and ultraviolet cut-on piece is housed, wavelength is made
Pass through greater than 420nm visible light.According to the kinetic curve of catalytic degradation methyl orange dye, to assess prepared photochemical catalyst
Visible light catalytic performance.The methyl orange solution for weighing 100 milliliters of concentration 20mg/L of 0.1g photochemical catalyst addition is placed in beaker, will
Beaker is placed on dark place with magnetic stirrer 30 minutes.Under above-mentioned radiation of light source, 3 milliliters were taken out every three minutes instead
Solution is answered, is centrifuged (1500rpm, 3 minutes), upper transparent liquid is taken out, its suction is tested with visible-ultraviolet specrophotometer
Luminosity.
Embodiment 3
Cotton fabric it is cation-modified: weigh 2 grams of cotton fabric, bath raio 1:30, by concentration be 50g/L weigh the chloro- 2- hydroxyl of 3-
3 grams of hydroxypropyltrimonium chloride, and claim 0.9 gram of 30g/L sodium hydroxide, it is put into conical flask.In oscillation overflow dyeing machine at 80 DEG C
Oscillation one hour or so is washed with distillation, 60 DEG C of baking oven drying.
Cotton Fabric: the cotton after will be cation-modified is added in the modified water-soluble glue of auto-dope stannic oxide, two
Leaching two is rolled, pick-up 100%, after slight washing, 60 DEG C of baking oven drying.
Fig. 6 is cotton fabric SEM figure, wherein (1) original cloth；(2) original cloth；(3) cotton that doping stannic oxide arranges；(4) it mixes
The cotton that miscellaneous stannic oxide arranges.It is found that flat belt-like structure when the form of fiber, has turnover to distort, meets the shape of cotton fiber
Looks feature.Cotton fiber is arranged, surface is covered with photochemical catalyst, there is the particle assembled on a small quantity, and it is whole to show that photochemical catalyst has succeeded
Manage fiber surface.
Fig. 7 is the Fourier Transform Infrared Spectroscopy figure of cotton fabric, wherein (a) SnO2The cotton fabric that-x is arranged；(b) original is knitted
Object as can be seen from the figure can have apparent characteristic peaks by auto-dope stannic oxide, these different peaks are fabric glazings
Peak corresponding to the different groups of catalyst, in 3740cm-1There is a peak than other peak intensities, which is the hydroxyl pair of hydrogen bond
The characteristic peak answered.It is 1630cm- in wave number1Place is the characteristic peak of amide.It is 1316cm- in wave number1For the absorption wave of quaternary ammonium salt
Peak.It is 1654cm- in wave number1Place is the absorption peak that the in-plane bending of amino is drawn, and is 671cm- in wave number1The peak at place be because
Sn-O-Sn stretching vibration.(a) with (b) it has been found by contrast that in wave number 1258cm-1There is apparent new peak value, the peak in place
Peak value caused by C-H bending vibration as in methyl.Illustrate that cotton fabric is drawn under alkaline condition by the method for chemical modification
Enter quaternary ammonium ion.
Fig. 8 is the Visible Light Induced Photocatalytic kinetic curve of finishing of cotton textiles and raw cotton fabric to methylene blue, (a) modified lighting
The degradation rate variation of catalysis 90 minutes, (b) the degradation rate variation of original cloth photocatalysis 90 minutes.It can be seen from the figure that photocatalysis
Agent finish fabric is degraded in 90min and is finished.This aspect shows that photochemical catalyst successfully arranges upper cotton fabric, while also saying
Bright, finish fabric has significant visible light catalysis activity, passes through the oxidation-reduction of photo-generate electron-hole, the work of generation
The property degradable methylene blue dye of kind.As previously mentioned, light-catalyzed reaction is the chemical reaction on surface, textile has porous and big
Surface area, load nano-photocatalyst after, self-cleaning performance of fabric can be assigned.Again as seen from the figure, raw cotton fabric does not have light
The ability of degradation of methylene blue.
Embodiment 4
Experiment of fading can simulate the practical self-cleaning performance of fabric, be added dropwise after red wine on Fig. 9 fabric under visible optical radiation
Colour fading experimental result picture, wherein 1 be illumination 0h；2 be illumination 1.5h；3 be illumination 3h.
As can be seen from Figure 9 the cotton after photochemical catalyst arranges (right side), red wine color above are got over increase with time
Come more shallow.And it is essentially unchanged not arrange cotton (left side) red wine color.Stannic oxide catalyst of the cotton on the right in doping as a result,
Under effect, spot can be decomposed, makes cotton fabric that there is self-cleaning function.
Embodiment 5
It prepares doping stannic oxide crystal: weighing suitable glass putty 0.36g (0.003mol) and stannic chloride pentahydrate 0.7g
(0.002mol) is added 60mL distilled water, is added in the stainless steel cauldron with polytetrafluoroethyllining lining after stirring, in baking oven
180 DEG C of high temperature bake for 24 hours, after cooling 5h, remove supernatant liquor, and lower sediment is placed in centrifuge tube, and 10000rpm is centrifuged 5min,
8mL distilled water is added in taking precipitate, washes 1 time, and 8mL ethyl alcohol is added, after carrying out washing 3 times to precipitating, 10000rpm centrifugation
Precipitating is placed in 60 DEG C of baking oven and dries 30min by 5min, is placed in grinding in the container of grinding, obtains the doping stannic oxide
Crystal；
The preparation auto-dope stannic oxide hydrosol: weighing 0.5g doping stannic oxide crystal and be added into 50mL water,
800rpm stirs 10min to get the auto-dope stannic oxide aqueous solution；
Cotton fabric it is cation-modified: weigh 2 grams of cotton fabric, bath raio 1:30, by concentration be 50g/L weigh the chloro- 2- hydroxyl of 3-
3 grams of hydroxypropyltrimonium chloride, and claim 0.9 gram of 30g/L sodium hydroxide, it is put into conical flask.In oscillation overflow dyeing machine at 80 DEG C
Oscillation one hour or so is washed with distillation, 60 DEG C of baking oven drying.
Cotton Fabric: the cotton after will be cation-modified is added in the modified water-soluble glue of auto-dope stannic oxide, two
Leaching two is rolled, pick-up 100%, after slight washing, 60 DEG C of baking oven drying, according to the power of catalytic degradation methylene blue dye
Curve is learned, to assess prepared photochemical catalyst visible light catalytic performance, measurement result is shown in that Figure 10, Tu10Zhong, (a) modified cloth mix
The variation of 90 minutes degradation rates of miscellaneous stannic oxide hydrosol modified photocatalytic, (c) the modified cloth doping stannic oxide hydrosol does not change
Property catalysis 90 minutes photodegradation rate variation, (d) 90 minutes photodegradation rates of original cloth doping stannic oxide hydrosol Modified catalytic
Variation.
Embodiment 6
It prepares doping stannic oxide crystal: weighing suitable glass putty 0.36g (0.003mol) and stannic chloride pentahydrate 0.7g
(0.002mol) is added 60mL distilled water, is added in the stainless steel cauldron with polytetrafluoroethyllining lining after stirring, in baking oven
180 DEG C of high temperature bake for 24 hours, after cooling 5h, remove supernatant liquor, and lower sediment is placed in centrifuge tube, and 10000rpm is centrifuged 5min,
8mL distilled water is added in taking precipitate, washes 1 time, and 8mL ethyl alcohol is added, after carrying out washing 3 times to precipitating, 10000rpm centrifugation
Precipitating is placed in 60 DEG C of baking oven and dries 30min by 5min, is placed in grinding in the container of grinding, obtains the doping stannic oxide
Crystal；
The preparation auto-dope stannic oxide hydrosol: 3, the 4- dihydroxyphenyl acetic acid of 8mg is weighed, 50mL distilled water is dissolved into
In, 10min is stirred under the conditions of 50KHz, 30 DEG C of ultrasonic treatments 5min, magnetic stirring apparatus 700rpm, and 0.5g is added and adulterates titanium dioxide
Tin crystal, 800rpm stir 10min to get the auto-dope stannic oxide hydrosol.
Cotton fabric it is cation-modified: weigh 2 grams of cotton fabric, bath raio 1:30, by concentration be 50g/L weigh the chloro- 2- hydroxyl of 3-
3 grams of hydroxypropyltrimonium chloride, and claim 0.9 gram of 30g/L sodium hydroxide, it is put into conical flask.In oscillation overflow dyeing machine at 80 DEG C
Oscillation one hour or so is washed with distillation, 60 DEG C of baking oven drying.
Cotton Fabric: the cotton after will be cation-modified is added in the modified water-soluble glue of auto-dope stannic oxide, two
Leaching two is rolled, pick-up 100%, after slight washing, 60 DEG C of baking oven drying, according to the power of catalytic degradation methylene blue dye
Curve is learned, to assess prepared photochemical catalyst visible light catalytic performance, measurement result is shown in Figure 10.
From Figure 10 it can clearly be seen that with glass putty and tin tetrachloride according to a certain percentage straight hydro-thermal reaction connect prepare oxygen sky
The stannic oxide crystal of position is modified with 3,4- dihydroxyphenyl acetic acid, improves the stability of colloidal sol, in conjunction with cotton fabric cation
It is modified, increase the electrostatic attraction of the stannic oxide hydrosol and fabric, improve nanoparticle and fabric binding force, improves fastness, it will
The modified or doping stannic oxide hydrosol is not modified cotton, and finish fabric visible light catalysis activity reduces.
The present invention successfully prepares the auto-dope stannic oxide hydrosol using hydro-thermal method, preferably four chlorinations of glass putty and crystallization out
The molar ratio of tin is 3:2, and the auto-dope stannic oxide of preparation is rutile-type, does not find other miscellaneous peaks, illustrates that Bivalent Tin enters
Lattice；TEM test shows that the partial size about 5nm of the auto-dope stannic oxide of preparation, photoelectricity current test show auto-dope titanium dioxide
The separative efficiency of the photo-generate electron-hole of tin is higher.The storage stability of auto-dope stannic oxide is good, after storage 3 months, catalysis
Activity does not reduce.
About auto-dope stannic oxide colloidal sol preparation method, conventional method in that art is that glass putty and tin tetrachloride are first disproportionated instead
Straight hydro-thermal reaction connects the titanium dioxide for preparing Lacking oxygen according to a certain percentage for Ying Houzai hydro-thermal, present invention glass putty and tin tetrachloride
Tin, surface have a large amount of hydroxyl, and the present invention provides a kind of preparation method of auto-dope stannic oxide hydrosol, with glass putty and four
Straight hydro-thermal reaction connects the stannic oxide crystal for preparing Lacking oxygen to stannic chloride according to a certain percentage, with 3,4- dihydroxyphenyl acetic acid
Modification, improves the stability of colloidal sol, cation-modified in conjunction with cotton fabric, and the electrostatic for increasing the stannic oxide hydrosol and fabric draws
Power improves nanoparticle and fabric binding force, improves fastness.
A kind of auto-dope stannic oxide hydrosol has been made in the present invention, is used for finishing of cotton textiles, and providing cotton fabric is significant
While self-cleaning performance, nanoparticle and fabric binding force can be improved, improves fastness.
It should be noted that the above examples are only used to illustrate the technical scheme of the present invention and are not limiting, although referring to preferable
Embodiment describes the invention in detail, those skilled in the art should understand that, it can be to technology of the invention
Scheme is modified or replaced equivalently, and without departing from the spirit and scope of the technical solution of the present invention, should all be covered in this hair
In bright scope of the claims.
Claims (9)
1. a kind of preparation method of the doping stannic oxide hydrosol, it is characterised in that: including,
It prepares doping stannic oxide crystal: weighing suitable glass putty and stannic chloride pentahydrate, distilled water dissolution is added, adds after stirring
Enter into the stainless steel cauldron with polytetrafluoroethyllining lining, baked for 24 hours in 180 DEG C of high temperature of baking oven, after cooling 5h, removes upper layer
Clear liquid, lower sediment are placed in centrifuge tube, and after 10000rpm is centrifuged 5min, taking precipitate is washed 1 time, and dehydrated alcohol is added, right
It washing of precipitate 3 times, after 10000rpm is centrifuged 5min, takes to be deposited in baking oven and dry, grind, obtain doping stannic oxide crystal；
The preparation auto-dope stannic oxide hydrosol: weighing 3, the 4- dihydroxyphenyl acetic acid of 8mg, be dissolved into 50mL distilled water,
Be ultrasonically treated 5min, magnetic stirrer 10min, be added 0.5g described in doping stannic oxide crystal, stir 10min to get
The auto-dope stannic oxide hydrosol.
2. the preparation method of the doping stannic oxide hydrosol as described in claim 1, it is characterised in that: dioxy is adulterated in the preparation
Change tin crystal, wherein the molar ratio of glass putty and stannic chloride pentahydrate is 3:2~3.
3. the preparation method of the doping stannic oxide hydrosol as claimed in claim 1 or 2, it is characterised in that: the glass putty and knot
The molar ratio of brilliant tin tetrachloride is 3:2.
4. the preparation method of the doping stannic oxide hydrosol as described in claim 1, it is characterised in that: described take is deposited in baking oven
Middle drying, wherein oven temperature is 60 DEG C, and the drying and processing time is 30min.
5. the preparation method of the doping stannic oxide hydrosol as described in claim 1, it is characterised in that: the preparation auto-dope two
The tin oxide hydrosol, wherein sonification power 50KHz, treatment temperature are 30 DEG C.
6. the preparation method of the doping stannic oxide hydrosol as described in claim 1, it is characterised in that: the magnetic stirring apparatus stirs
Mix 10min, wherein speed of agitator 700rpm.
7. the preparation method of the doping stannic oxide hydrosol as described in claim 1, it is characterised in that: described in the addition 0.5g
Doping stannic oxide crystal stirs 10min to get the auto-dope stannic oxide hydrosol, wherein it stirs as mechanical stirring,
Speed of agitator is 800rpm.
8. a kind of preparation method of the auto-dope stannic oxide hydrosol as described in any one of claim 1,2,4,5,6,7 is made
The doping stannic oxide hydrosol.
9. application of the auto-dope stannic oxide hydrosol as claimed in claim 8 in cotton fabric automatically cleaning.
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