CN110436792A - A method of preparing the quartz capillary with titanium dioxide nano-particle coating - Google Patents
A method of preparing the quartz capillary with titanium dioxide nano-particle coating Download PDFInfo
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- CN110436792A CN110436792A CN201910771950.7A CN201910771950A CN110436792A CN 110436792 A CN110436792 A CN 110436792A CN 201910771950 A CN201910771950 A CN 201910771950A CN 110436792 A CN110436792 A CN 110436792A
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- titanium dioxide
- dioxide nano
- particle
- quartz capillary
- capillary
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Classifications
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
- C03C17/23—Oxides
- C03C17/25—Oxides by deposition from the liquid phase
- C03C17/256—Coating containing TiO2
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/21—Oxides
- C03C2217/212—TiO2
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
- C03C2218/111—Deposition methods from solutions or suspensions by dipping, immersion
Abstract
A kind of method preparing the quartz capillary with titanium dioxide nano-particle coating of the invention belongs to the technical field of inorganic functional material preparation process.Titanium dioxide nano-particle dispersion by average grain diameter less than 5nm is ultrasonically treated to being uniformly dispersed in a solvent, and obtaining concentration is 20~150g/L titanium dioxide nano-particle colloidal sol；Quartz capillary deionized water to be rinsed 10 minutes, naturally dry is placed on syringe pump, and titanium dioxide nano-particle colloidal sol is injected into capillary with microsyringe and is coated, after the completion of coating, dry 2 hours under the conditions of constant temperature and humidity.Preparation process of the present invention is easy, and preparation condition is mild, is conducive to industrialized production.And without introducing the additives such as any template, pore-foaming agent in preparation process, the quartz capillary column obtained with titanium dioxide nano-particle coating solid phase microextraction and in terms of be with a wide range of applications.
Description
Technical field
The invention belongs to the technical fields of inorganic functional material preparation process.Particularly relate to titanium dioxide nano-particle
Coat quartz capillary.
Background technique
Titanium dioxide nano-particle is extensive with its good absorption property, catalytic performance, nontoxicity and biocompatibility
Applied to fields such as absorption, catalysis, photosensitive material, coating and cosmetics, in sewage, the improvement of waste water from dyestuff, phosphorylation egg
White separation and enrichment, the degradation of organic pollutant and the diagnoses and treatment of disease etc. have broad application prospects.In recent years
Come, filled type capillary monolithic column is simple with its preparation as microreactor, continuous flow is strong, solvent good compatibility, selection
The advantages that property absorption property is high is widely used in the fields such as biological detection, chemical technology, food processing, environmental improvement.
The main organic and inorganic compound two major classes of the raw material of filled type capillary monolithic column reported at present.Its
In, more the most commonly used is ionic liquid, organic high molecular compound such as polymethyl methacrylates, isopropyl in organic compound
Acrylamide etc..Then common metal or nonmetal oxide, inorganic nano material etc. in inorganic compound.As Huang et al. is logical
It crosses Microwave Emulsifier-Free Polymerization and acts on obtained MOF- organic polymer mixing capillary column.The stationary phase of the capillary column is porous, organometallic
Framework compound MIL-101 (Cr) and organic high molecular polymer dimethacrylate diethyl alcohol ester, methyl propane sulfonic acid butyl ester and
2- acrylamide-2-methylpro panesulfonic acid.Capillary column obtained shows high osmosis, and can efficiently separate dimethylbenzene,
Chlorotoluene, polycyclic aromatic hydrocarbon and trypsin digestion BSA polypeptide (Analytica Chimica Acta, 2013,779,96-
103).Feng et al. is in the mixed solution containing butyl titanate, tetramethoxy-silicane, glycerol, ethyl alcohol, acetic acid and polyethylene glycol
SiO is made by sol-gel method2/TiO2Colloidal sol.It is filled into capillary as syringe colloidal sol by obtained by, at 120 DEG C
Dry 3 hours.By capillary column obtained be used for specific enrichment polypeptide phosphate (Analytical Chemistry, 2012,
84,7763-7770).Partial size is less than the titanium dioxide nano-particle of 5nm since particle size is small, and surface atom quantity increases, grain
The surface area and surface of son can increase, and enhance the adsorption capacity of ambient substance, and directly using titanium dioxide nano-particle as
Raw material prepares capillary column currently without report.
Summary of the invention
It is raw material quartz capillary that the object of the present invention is to provide a kind of using superfine titanic oxide nanoparticle
Method.It is controllable, continuous flawless using the coating of titanium dioxide thickness of the deposition of quartz capillary inner wall made from this method.
Specific technical solution is as follows:
A method of the quartz capillary with titanium dioxide nano-particle coating is prepared, average grain diameter is less than 5nm
Titanium dioxide nano-particle dispersion in a solvent, be ultrasonically treated to being uniformly dispersed, obtain concentration be 20~150g/L titanium dioxide
Titanium nanoparticle sol；Quartz capillary deionized water is rinsed 10 minutes, naturally dry is placed on syringe pump, and use is micro
Titanium dioxide nano-particle colloidal sol is injected into capillary and coats by sample injector, after the completion of coating, in constant temperature and humidity condition
2 hours of lower drying.
The concentration of the titanium dioxide nano-particle colloidal sol is preferably 80~150g/L.When titanium dioxide nano-particle is molten
Gum concentration will lead to quartz capillary inner wall coating of titanium dioxide thickness when being greater than 150g/L is blocked up and separate and go out with inner wall
Existing slight crack；When concentration is less than 80g/L, the coating of titanium dioxide of quartz capillary inner wall is thinner, needs repeatedly to coat.
The solvent can be water, alkane or alcohol-water mixture etc..
Described titanium dioxide nano-particle colloidal sol is injected into capillary with microsyringe coats, and preferably 10
It completes within~20 minutes.
The constant temperature and humidity condition, preferred range is at 30~60 DEG C；It is preferred that humidity range is 45%~65%.
Titanium dioxide nano-particle of the present invention using average grain diameter less than 5nm coats quartz capillary,
The utility model has the advantages that
1, the titanium dioxide nano-particle of crystallization of the present invention using average grain diameter less than 5nm, avoids conventional sol
Required high temperature crystallization process in gel process.
2, the titanium dioxide nano-particle uniform coating thickness of the obtained quartz capillary inner wall of the present invention is controllable, continuously nothing is split
Trace, property are stablized, and are conducive to separate and be enriched with detection.
3, preparation process of the present invention is easy, and preparation condition is mild, is conducive to industrialized production.And without drawing in preparation process
Enter the additives such as any template, pore-foaming agent, the quartz capillary column obtained with titanium dioxide nano-particle coating is solid
Phase extraction and microreactor etc. are with a wide range of applications.
Detailed description of the invention:
Fig. 1 is the X-ray diffraction spectrogram of titanium dioxide nano-particle dried powder made from embodiment 1.
Fig. 2 is that the cross section of the quartz capillary inner wall obtained with titanium dioxide nano-particle coating of embodiment 1 is swept
Retouch electron microscope.
Fig. 3 is that the cross section of the quartz capillary inner wall obtained with titanium dioxide nano-particle coating of embodiment 2 is swept
Retouch electron microscope.
Fig. 4 is that the cross section of the quartz capillary inner wall obtained with titanium dioxide nano-particle coating of embodiment 3 is swept
Retouch electron microscope.
Fig. 5 is that the cross section of the quartz capillary inner wall obtained with titanium dioxide nano-particle coating of embodiment 4 is swept
Retouch electron microscope.
Fig. 6 is that the cross section of the quartz capillary inner wall obtained with titanium dioxide nano-particle coating of embodiment 6 is swept
Retouch electron microscope.
Specific embodiment
Embodiment 1
36mL butyl titanate is added in the in the mixed solvent that 180mL hexamethylene and ethyl alcohol volume ratio are 1:1.It stirs evenly
Afterwards, then by volume butyl titanate: 9mL concentrated hydrochloric acid (36%~38%) is added in concentrated hydrochloric acid=1:0.25 ratio.It is warming up to
It flows back 10 hours after boiling.Under stiring, ethyl alcohol is added dropwise dropwise extremely into the product (light yellow transparent liquid) after back flow reaction
Product precipitating completely, washing, centrifugation, dry titanium dioxide nano-particle powder.Precise 0.8g is dry, and titanium dioxide is received
Rice corpuscles powder is dispersed in 10mL deionized water, and for ultrasonic 10min to being uniformly dispersed, obtaining concentration is that 80g/L titanium dioxide is received
Rice corpuscles colloidal sol.
It takes 10cm quartz capillary to be placed on syringe pump, 200 μ L colloidal sols is accurately measured using microsyringe, in syringe pump
Promotion under colloidal sol be all injected into quartz capillary in 10 minutes coat.It is 60 in temperature after the completion of coating
DEG C humidity dry 2 hours under conditions of being 65%.Wherein, quartz capillary is rinsed 10 minutes with deionized water in advance, natural
It dries.
Fig. 1 is the X-ray diffraction spectrogram of titanium dioxide nano-particle dried powder obtained.Illustrate gained titanium dioxide
Nanoparticle is anatase phase titanium dioxide, and average grain diameter is about 5nm.Fig. 2, which is that embodiment 1 is obtained, has nano titania
The cross-sectional scans electron microscope of the quartz capillary inner wall of particle coating.Illustrate the coating of the quartz capillary inner wall by titanium dioxide
Titanium self-assembly is constituted, coating uniform, continuous, flawless, and thickness is about 135nm.
Embodiment 2
36mL butyl titanate is added with the in the mixed solvent that ethyl alcohol volume ratio is 1:1 in 180mL hexamethylene to stir evenly
Afterwards, then by volume butyl titanate: 9mL concentrated hydrochloric acid (36%~38%) is added in concentrated hydrochloric acid=1:0.25 ratio.It is warming up to
It flows back 10 hours after boiling.Under stiring, ethyl alcohol is added dropwise dropwise extremely into the product (light yellow transparent liquid) after back flow reaction
Product precipitating completely, washing, centrifugation, dry titanium dioxide nano-particle powder.Precise 0.2g is dry, and titanium dioxide is received
Rice corpuscles powder is dispersed in 10mL deionized water, and for ultrasonic 10min to being uniformly dispersed, obtaining concentration is that 20g/L titanium dioxide is received
Rice corpuscles colloidal sol.
It takes 10cm quartz capillary to be placed on syringe pump, 200 μ L colloidal sols is accurately measured using microsyringe, in syringe pump
Promotion under colloidal sol be all injected into quartz capillary in 10 minutes coat.It is 30 in temperature after the completion of coating
DEG C humidity dry 2 hours under conditions of being 65%.Wherein, quartz capillary is rinsed 10 minutes with deionized water in advance, natural
It dries.
Compared with embodiment 1, the concentration of titanium dioxide nano-particle colloidal sol is reduced to 20g/L.Fig. 3 is made for embodiment 2
The quartz capillary inner wall with titanium dioxide nano-particle coating cross-sectional scans electron microscope.Work as titanium dioxide nano granule
When the concentration of sub- colloidal sol is reduced to 20g/L, the coating layer thickness that quartz capillary inner wall is made of titanium dioxide nano-particle changes
Obviously.It can be seen that thickness is reduced, average thickness is about 54nm.
Embodiment 3
36mL butyl titanate is added in the in the mixed solvent that 180mL hexamethylene and ethyl alcohol volume ratio are 1:1.It stirs evenly
Afterwards, then by volume butyl titanate: 9mL concentrated hydrochloric acid (36%~38%) is added in concentrated hydrochloric acid=1:0.25 ratio.It is warming up to
It flows back 10 hours after boiling.Under stiring, ethyl alcohol is added dropwise dropwise extremely into the product (light yellow transparent liquid) after back flow reaction
Product precipitating completely, washing, centrifugation, dry titanium dioxide nano-particle powder.Precise 1.5g is dry, and titanium dioxide is received
Rice corpuscles powder is dispersed in 10mL deionized water, and for ultrasonic 10min to being uniformly dispersed, obtaining concentration is 150g/L titanium dioxide
Nanoparticle sol.
It takes 10cm quartz capillary to be placed on syringe pump, 200 μ L colloidal sols is accurately measured using microsyringe, in syringe pump
Promotion under colloidal sol be all injected into quartz capillary in 20 minutes coat.It is 50 in temperature after the completion of coating
DEG C humidity dry 2 hours under conditions of being 45%.Wherein, quartz capillary is rinsed 10 minutes with deionized water in advance, natural
It dries.
Compared with embodiment 1, the concentration of titanium dioxide nano-particle colloidal sol is increased to 150g/L.Fig. 4 is made for embodiment 3
The quartz capillary inner wall with titanium dioxide nano-particle coating cross-sectional scans electron microscope.It can be seen that when two
When the concentration of titanium oxide nanoparticles colloidal sol is increased to 150g/L, quartz capillary inner wall is made of titanium dioxide nano-particle
It is coating even uniform, continuous flawless, and thickness increases to 350nm.
Embodiment 4
36mL butyl titanate is added in the in the mixed solvent that 180mL hexamethylene and ethyl alcohol volume ratio are 1:1.It stirs evenly
Afterwards, then by volume butyl titanate: 9mL concentrated hydrochloric acid (36%~38%) is added in concentrated hydrochloric acid=1:0.25 ratio.It is warming up to
It flows back 10 hours after boiling.Under stiring, ethyl alcohol is added dropwise dropwise extremely into the product (light yellow transparent liquid) after back flow reaction
Product precipitating completely, washing, centrifugation, dry titanium dioxide nano-particle powder.Precise 0.8g is dry, and titanium dioxide is received
Rice corpuscles powder is dispersed in 10mL ethyl alcohol, and for ultrasonic 10min to being uniformly dispersed, obtaining concentration is 80g/L titanium dioxide nano granule
Sub- colloidal sol.
It takes 10cm quartz capillary to be placed on syringe pump, 200 μ L colloidal sols is accurately measured using microsyringe, in syringe pump
Promotion under colloidal sol be all injected into quartz capillary in 10 minutes coat.It is 60 in temperature after the completion of coating
DEG C humidity dry 2 hours under conditions of being 65%.Wherein, quartz capillary is rinsed 10 minutes with deionized water in advance, natural
It dries.
Compared with embodiment 1, the dispersion solvent of titanium dioxide nano-particle colloidal sol is changed to ethyl alcohol.Fig. 5 is made for embodiment 4
The quartz capillary inner wall with titanium dioxide nano-particle coating cross-sectional scans electron microscope.It can be seen that quartzy
Out-of-flatness is omited on the coating of titanium dioxide surface of capillary tube inner wall, but continuous flawless, and thickness is about 120nm.
Following example 5~6 are reference examples, are not belonging to protection scope of the present invention.
Embodiment 5
36mL butyl titanate is added in the in the mixed solvent that 180mL hexamethylene and ethyl alcohol volume ratio are 1:1.It stirs evenly
Afterwards, then by volume butyl titanate: 9mL concentrated hydrochloric acid (36%~38%) is added in concentrated hydrochloric acid=1:0.25 ratio.It is warming up to
It flows back 10 hours after boiling.Under stiring, ethyl alcohol is added dropwise dropwise extremely into the product (light yellow transparent liquid) after back flow reaction
Product precipitating completely, washing, centrifugation, dry titanium dioxide nano-particle powder.Precise 0.02g is dry, and titanium dioxide is received
Rice corpuscles powder is dispersed in 10mL ethyl alcohol, and for ultrasonic 10min to being uniformly dispersed, obtaining concentration is 2g/L titanium dioxide nano granule
Sub- colloidal sol.
It takes 10cm quartz capillary to be placed on syringe pump, 200 μ L colloidal sols is accurately measured using microsyringe, in syringe pump
Promotion under colloidal sol be all injected into quartz capillary in 10 minutes coat.It is 60 in temperature after the completion of coating
DEG C humidity dry 2 hours under conditions of being 65%.Wherein, quartz capillary is rinsed 10 minutes with deionized water in advance, natural
It dries.
Compared with embodiment 1, the solubility of titanium dioxide nano-particle ethyl alcohol colloidal sol is changed to 2g/L.Due to nano titania
The concentration of particle ethyl alcohol colloidal sol is too low, and reduces the probability of titanium dioxide nano-particle self assembly in ethyl alcohol colloidal sol, finally
Apparent coating of titanium dioxide is not observed in quartz capillary inner wall.
Embodiment 6
36mL butyl titanate is added in the in the mixed solvent that 180mL hexamethylene and ethyl alcohol volume ratio are 1:1.It stirs evenly
Afterwards, then by volume butyl titanate: 9mL concentrated hydrochloric acid (36%~38%) is added in concentrated hydrochloric acid=1:0.25 ratio.It is warming up to
It flows back 10 hours after boiling.Under stiring, ethyl alcohol is added dropwise dropwise extremely into the product (light yellow transparent liquid) after back flow reaction
Product precipitating completely, washing, centrifugation, dry titanium dioxide nano-particle powder.Precise 2.0g is dry, and titanium dioxide is received
Rice corpuscles powder is dispersed in 10mL ethyl alcohol, and for ultrasonic 10min to being uniformly dispersed, obtaining concentration is 200g/L nano titania
Colloidal sol.
It takes 10cm quartz capillary to be placed on syringe pump, 200 μ L colloidal sols is accurately measured using microsyringe, in syringe pump
Promotion under colloidal sol be all injected into quartz capillary in 10 minutes coat.It is 60 in temperature after the completion of coating
DEG C humidity dry 2 hours under conditions of being 65%.Wherein, quartz capillary is rinsed 10 minutes with deionized water in advance, natural
It dries.
Compared with embodiment 1, the concentration of titanium dioxide nano-particle colloidal sol is increased to 200g/L.Fig. 6 is made for embodiment 6
The quartz capillary inner wall with titanium dioxide nano-particle coating cross-sectional scans electron microscope.Work as titanium dioxide nano granule
When the concentration of sub- colloidal sol is increased to 200g/L, it can be seen that quartz capillary inner wall was made of titanium dioxide nano-particle
Coating layer thickness increases to 420nm, and since the excessive concentration of titanium dioxide nano-particle colloidal sol causes coating layer thickness blocked up, part is applied
Layer is separated with quartz capillary inner wall.
By above embodiments 5~6 as it can be seen that when the excessive concentration of titanium dioxide nano-particle colloidal sol or it is too low when, in quartz
Capillary tube inner wall cannot continuous crackless coating of titanium dioxide.
Claims (5)
1. a kind of method for preparing the quartz capillary with titanium dioxide nano-particle coating, by average grain diameter less than 5nm's
Titanium dioxide nano-particle disperses in a solvent, to be ultrasonically treated to being uniformly dispersed, and obtaining concentration is 20~150g/L titanium dioxide
Nanoparticle sol；By quartz capillary with deionized water rinse 10 minutes, naturally dry is placed on syringe pump, with it is micro into
Titanium dioxide nano-particle colloidal sol is injected into capillary and coats by sample device, after the completion of coating, under the conditions of constant temperature and humidity
Dry 2 hours.
2. a kind of method for preparing the quartz capillary with titanium dioxide nano-particle coating according to claim 1,
It is characterized in that, the concentration of the titanium dioxide nano-particle colloidal sol is 80~150g/L.
3. a kind of method for preparing the quartz capillary with titanium dioxide nano-particle coating according to claim 1,
It is characterized in that, the solvent is water, alkane or alcohol-water mixture.
4. a kind of method for preparing the quartz capillary with titanium dioxide nano-particle coating according to claim 1,
It is characterized in that, described titanium dioxide nano-particle colloidal sol is injected into capillary with microsyringe coats, In
It completes within 10~20 minutes.
5. a kind of quartz capillary prepared with titanium dioxide nano-particle coating according to any one of claims 1 to 4
Method, which is characterized in that the constant temperature and humidity condition, refer to temperature range 30~60 DEG C, humidity range 45%~
65% condition.
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Application publication date: 20191112 |