CN108751168A - A kind of preparation method of the flower-shaped diamond shape titanium dioxide/graphene composite material of Detitanium-ore-type for photoproduction cathodic protection - Google Patents
A kind of preparation method of the flower-shaped diamond shape titanium dioxide/graphene composite material of Detitanium-ore-type for photoproduction cathodic protection Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
- C01G23/0536—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing chloride-containing salts
- C01G23/0538—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing chloride-containing salts in the presence of seeds
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F13/00—Inhibiting corrosion of metals by anodic or cathodic protection
- C23F13/02—Inhibiting corrosion of metals by anodic or cathodic protection cathodic; Selection of conditions, parameters or procedures for cathodic protection, e.g. of electrical conditions
- C23F13/06—Constructional parts, or assemblies of cathodic-protection apparatus
- C23F13/08—Electrodes specially adapted for inhibiting corrosion by cathodic protection; Manufacture thereof; Conducting electric current thereto
- C23F13/12—Electrodes characterised by the material
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
Abstract
The invention discloses a kind of preparation methods of the flower-shaped diamond shape titanium dioxide/graphene composite material of the Detitanium-ore-type for photoproduction cathodic protection, belong to anti-corrosion material preparation field.First graphene oxide dispersion is added in titanium tetrachloride solution by the present invention, pass through heating by titanium source of titanium tetrachloride, it is nanocrystalline that the techniques such as calcining grow anatase titanium dioxide on graphene, then to addition titanium dioxide crystal seed/graphene composite material in titanium precursors solution, and carry out hydro-thermal reaction, under hydrothermal condition, the presence of crystal seed makes anatase titanium dioxide fast-growth, and the formation of the flower-shaped shape of titanium dioxide can be effectively facilitated, finally obtain the flower-shaped diamond shape titanium dioxide/graphene photoproduction cathodic protection material of Detitanium-ore-type, the photoproduction cathodic protection material electricity conversion is good, anti-corrosion effect is good, and it is with a wide range of applications.
Description
Technical field
The invention belongs to anti-corrosion material preparation fields, and in particular to a kind of Detitanium-ore-type for photoproduction cathodic protection is flower-shaped
The preparation method of diamond shape titanium dioxide/graphene composite material.
Background technology
Metal material especially steel structure is in use it occur frequently that corrosion phenomenon, causes environmental pollution, resource
Waste, seriously endangers the work and life of people, and also result in massive losses to national economy.Therefore, metal protection seems
It is particularly important.The method of metal protection mainly has sacrificial anode protection, impressed current method and photo-catelectrode protection method etc. at present.Photoproduction is cloudy
Pole protection be a kind of novel anticorrosion technology developed in recent years, have not sacrificial anode, do not consume electric energy, it is cheap and
Advantages of environment protection.
In numerous photoproduction cathodic protection materials, titanium dioxide has the features such as non-toxic, stability is good, thus all the time all
It is the hot spot of photoelectric field research；In recent years, graphene is also accounted for due to its high electric conductivity in photoproduction cathodic protection field
According to one seat.Titanium dioxide/graphene composite material combines the advantages of both titanium dioxide and graphene, has excellent
Photoproduction cathodic protection performance.Its basic principle：Under light illumination, the electrons on the titanium dioxide in composite material are excited,
Titanium dioxide be stimulated generate light induced electron transit to conduction band from its valence band, due to the good electric conductivity of graphene, as electronics
A large amount of electronics is rapidly migrated to stainless steel electrode so that on stainless steel electrode by the bridge of transmission from the conduction band of titanium dioxide
Electron density increase, current potential decreases below its corrosion potential, it is suppressed that corrosion of metal, to make stainless steel obtain
It is effectively protected.Chinese patent (application number 201510153765.3) provides a kind of flower-shaped titanium dioxide/graphite of rutile-type
The preparation method of alkene composite material, the technology show the superiority of flower-like structure titanium dioxide, i.e., the specific surface area of bigger and
Electron-transport efficiency；However, compared to anatase titanium dioxide, the photoresponse ability and photocathode of rutile titanium dioxide
Barrier propterty is weaker.However Chinese patent (application number 201410355247.5) provides a kind of anatase titanium dioxide/stone
The preparation method of black alkene composite material, but conventional anatase titanium dioxide crystal form, and the ratio table of crystal can only be made in it
Area is not big enough.Therefore, it synthesizes a kind of flower-shaped diamond shape titanium dioxide/graphene composite material of Detitanium-ore-type and shows important especially.
Invention content
The problem of for background technology, the present invention provides a kind of Detitanium-ore-type flowers for photoproduction cathodic protection
Shape diamond shape composite titania material, this method preparation process is simple, and photoproduction cathodic protection is efficient.
The present invention provides a kind of preparation sides of the above-mentioned flower-shaped diamond shape titanium dioxide/graphene composite material of Detitanium-ore-type
Method, steps are as follows for specific features：
1, titanium tetrachloride solution is added into graphene oxide dispersion, after being sufficiently stirred at 60~80 DEG C heating 1~
3h after being cooled to room temperature, is washed to neutrality, and the sample after washing is dry at 60~80 DEG C, and the nitrogen at 400~600 DEG C
Atmosphere encloses 1~3h of middle calcining to get to anatase titanium dioxide crystal seed/graphene composite material,
Wherein, the mass concentration of graphene oxide is 1~2mg/mL in graphene oxide dispersion, titanium tetrachloride solution
Molar concentration is 2.5~4.0mol/L；Graphene oxide dispersion and the volume ratio of titanium tetrachloride solution are 45~70:1~2.
2,1~2mL titanium tetrachloride solutions are added in the hydrochloric acid solution that molar concentration is 4.0~6.0mol/L and titanium is made
Anatase titanium dioxide crystal seed/the graphene composite material obtained in step 1, ultrasonic disperse, mixing is added in precursor solution
After uniformly, mixed dispersion liquid is transferred in water heating kettle, water heating kettle is moved in baking oven, hydro-thermal is anti-under the conditions of 150~180 DEG C
10~16h is answered, after being cooled to room temperature, filter cake is collected and simultaneously washs to neutrality, is dried at 60~80 DEG C to get to Detitanium-ore-type
Flower-shaped diamond shape titanium dioxide/graphene photoproduction cathodic protection material,
Wherein, the molar concentration of titanium tetrachloride solution is 2.5~4.0mol/L.
Beneficial effects of the present invention are as follows：
(1) anatase titanium dioxide of the invention that first grown on graphite oxide using titanium tetrachloride as titanium source is nanocrystalline, obtains
To anatase titanium dioxide crystal seed/graphene composite material, titanium precursors solution is then added again, can be used as titanium source in water
There is fast-growth the anatase titanium dioxide of regular shape, the present invention to utilize anatase on the basis of crystal seed under heat condition
Type titanium dioxide crystal seed induces the growth of anatase, to effectively facilitate the formation of the flower-shaped shape of titanium dioxide, finally obtains
The titanium dioxide/graphene composite material of flower-shaped diamond structure, due to the formation of the titanium dioxide of flower-shaped diamond structure, greatly
The specific surface area for increasing composite material improves photoresponse ability；
(2) present invention is with compared with conventional hydrothermal method, and simple for process, required operating procedure is few, efficient, in preparation process
The variable to be controlled is few, can improve product precision；
(3) graphene in composite material of the present invention can play lamella barrier due to the lamellar structure of itself to metal
Effect, avoids that metal is protected directly to contact with corrosive medium, and its high conductivity can promote the separation in light induced electron and hole.
Description of the drawings
Fig. 1 is the flower-shaped diamond shape titanium dioxide/graphene composite material X-ray diffraction of Detitanium-ore-type prepared by embodiment 1
Figure；
Fig. 2 is the flower-shaped diamond shape titanium dioxide/graphene composite material scanning electron microscope of Detitanium-ore-type prepared by embodiment 1
Figure；
Fig. 3 is the flower-shaped diamond shape titanium dioxide of Detitanium-ore-type obtained in embodiment 1 and comparative example 1, comparative example 2, comparative example 3
Titanium/graphene composite material photocurrent-time curve comparison diagram.
Specific implementation mode
Embodiment 1
1, the graphene oxide dispersion 60mL of 1mg/mL is taken, three-necked flask is moved into, 1mL titanium tetrachloride solutions are added dropwise, often
Temperature is lower to stir 2h, then moves into 60 DEG C of heat preservation 2h of baking oven, is washed after being cooled to room temperature, and the sample after washing is dry at 60 DEG C,
Sample after drying calcines 2h to get to anatase titanium dioxide crystal seed/graphene composite wood at 500 DEG C in nitrogen atmosphere
Material；
2,1mL titanium tetrachloride solutions and 30mL molar concentrations are mixed for the hydrochloric acid solution of 5.0mol/L, titanium precursor is made
Body aqueous solution adds 100mg anatase titanium dioxides nanosized seeds/graphene composite material, by hydro-thermal after being sufficiently stirred
Kettle moves in baking oven, and the hydro-thermal reaction 12h at 160 DEG C is washed after being cooled to room temperature, and the sample after washing is done at 60 DEG C
It is dry to get to the flower-shaped diamond shape titanium dioxide/graphene composite material of Detitanium-ore-type.
Embodiment 2
1, the graphene oxide dispersion 45mL of 1.5mg/mL is taken, three-necked flask is moved into, 1mL titanium tetrachloride solutions are added dropwise,
1h is stirred under room temperature, 60 DEG C of heat preservation 1h of baking oven is then moved into, is washed after being cooled to room temperature, it is dry at 60 DEG C of sample after washing, it does
Sample after dry calcines 1h to get to titanium dioxide crystal seed/graphene composite material at 400 DEG C in nitrogen atmosphere；
2,1mL titanium tetrachloride solutions and 30mL molar concentrations are mixed for the hydrochloric acid solution of 4.0mol/L, titanium precursor is made
Body aqueous solution adds 100mg anatase titanium dioxides nanosized seeds/graphene composite material, by hydro-thermal after being sufficiently stirred
Kettle moves in baking oven, and the hydro-thermal reaction 10h at 150 DEG C is washed after being cooled to room temperature, and the sample after washing is done at 60 DEG C
It is dry to get to the flower-shaped diamond shape titanium dioxide/graphene composite material of Detitanium-ore-type.
Embodiment 3
1, the graphene oxide dispersion 50mL of 1.8mg/mL is taken, three-necked flask is moved into, it is molten that 1.5mL titanium tetrachlorides are added dropwise
Liquid stirs 1.5h under room temperature, then moves into 70 DEG C of heat preservation 1.5h of baking oven, is washed after being cooled to room temperature, after washing at 70 DEG C of sample
It is dry, it is dry after sample 2h is calcined in nitrogen atmosphere at 500 DEG C to get to titanium dioxide crystal seed/graphene composite material；
2,1.5mL titanium tetrachloride solutions and 30mL molar concentrations are mixed for the hydrochloric acid solution of 5.0mol/L, before titanium is made
Body aqueous solution is driven, 100mg anatase titanium dioxides nanosized seeds/graphene composite material is added, by water after being sufficiently stirred
Hot kettle moves in baking oven, and the hydro-thermal reaction 13h at 165 DEG C, after being cooled to room temperature, centrifuge washing, the sample after washing is 70
It is dried to get to the flower-shaped diamond shape titanium dioxide/graphene composite material of Detitanium-ore-type at DEG C.
Embodiment 4
1, the graphene oxide dispersion 60mL of 2mg/mL is taken, three-necked flask is moved into, 2mL titanium tetrachloride solutions are added dropwise, often
Temperature is lower to stir 2h, then moves into 80 DEG C of heat preservation 2h of baking oven, is cooled to room temperature rear centrifuge washing, dry at 80 DEG C of sample after washing,
Sample after drying calcines 3h to get to titanium dioxide crystal seed/graphene composite material at 600 DEG C in nitrogen atmosphere；
2,2mL titanium tetrachloride solutions and 30mL molar concentrations are mixed for the hydrochloric acid solution of 6.0mol/L, titanium precursor is made
Body aqueous solution adds 100mg anatase titanium dioxides nanosized seeds/graphene composite material, by hydro-thermal after being sufficiently stirred
Kettle moves in baking oven, and the hydro-thermal reaction 16h at 180 DEG C is washed after being cooled to room temperature, and the sample after washing is done at 80 DEG C
It is dry to get to the flower-shaped diamond shape titanium dioxide/graphene composite material of Detitanium-ore-type.
Comparative example 1
The method that conventional method prepares anatase titanium dioxide/graphene composite material：
Graphene oxide is prepared using Hummers methods, graphene oxide is dissolved in ethyl alcohol, ultrasonic 2h obtains a concentration of
The graphene oxide solution of 3mg/mL；3.74g cetylamines are taken to be added to the water of 240mL absolute ethyl alcohol 1.3mL potassium chloride (0.1M)
In solution, ultrasonic 10min is placed on magnetic stirring apparatus and is stirred at room temperature, and 5.4mL isopropyl titanates are slowly dropped to mixed solution
In, 18h is reacted, then filtering reacting solution is washed 3 times repeatedly with ethyl alcohol, dry to obtain TiO 2 precursor；Take 1.6g bis-
Titania precursor body is dissolved in 20mL absolute ethyl alcohols and 10mL water, and 255 μ L ammonia spirits are added dropwise, mixed solution is transferred to hydro-thermal
180 DEG C of reaction 16h in reaction kettle, cooled and filtered, drying sample obtain titania nanoparticles；By 0.3g titanium dioxide
Nano particle is mixed into 20mL graphene oxide solutions (3mg/mL), and hydro-thermal is placed it in after ultrasonic 30min and after ammonium hydroxide is added
In reaction kettle, 180 DEG C of reaction 16h；Then it after reaction product being cooled to room temperature, filters and with the water on filter paper pipette samples surface
Divide simultaneously freeze-drying process；Finally by the sample after drying, 500 DEG C of heat treatment 2h are obtained in the tube furnace that argon gas atmosphere is protected
Anatase titanium dioxide/graphene composite material.
Comparative example 2
In embodiment 1, remove the process of graphene surface growth crystal seed in embodiment 1, other operations and 1 phase of embodiment
Together：
1,100mg graphite oxides, 15mL concentrated hydrochloric acids and 15mL deionized waters are added in water heating kettle, then 1mL tetra- is added dropwise
Titanium chloride solution moves to water heating kettle in baking oven after being sufficiently stirred, the hydro-thermal reaction 12h at 160 DEG C, after being cooled to room temperature,
Centrifuge washing, sample after washing are dried at 60 DEG C to get to titanium dioxide/oxidized graphite composite material；
2, titanium dioxide/oxidized graphite composite material is calcined to 2h at 500 DEG C to get to titanium dioxide in nitrogen atmosphere
Titanium/graphene composite material.
Comparative example 3
Anatase-type nanometer titanium dioxide：
It takes the titanium tetrachloride solution 20mL of 2.5mol/L in three-necked flask, takes the sodium hydroxide solution 60mL of 2.5mol/L
In dropping funel, sodium hydroxide solution, rate of addition 3mL/ are added dropwise into titanium tetrachloride solution in stirring at room temperature
Min continues to stir 30min after dripping, and system is warming up to 85 DEG C, maintains 2h, use after reaction salt acid for adjusting pH value to 5~
6, then filtering and washing, filter cake is dried at 80 DEG C to get to anatase-type nanometer titanium dioxide.
The titanium dioxide that can be seen that in Fig. 1 x-ray diffraction patterns in the composite material prepared by the present invention is anatase
Type titanium dioxide.
Can be seen that titanium dioxide in the composite material prepared by the present invention in Fig. 2 scanning electron microscope (SEM) photographs has unique flower
Shape diamond structure.This structure greatly improves the specific surface area of the composite material, and the structure is comparative example 1, comparative example 2
Do not have with the titanium dioxide in comparative example 3.
Antiseptic property is tested：The material prepared by 50mg embodiments 1, comparative example 1, comparative example 2 and comparative example 3 is taken, in 1mL
Abundant ultrasonic disperse in water, it is 1cm then to take 50 μ L homogeneous dispersions to be coated on area2304 stainless steel electrode of circle on, wait for
After its natural air drying, which is immersed in the sodium chloride solution that Solute mass fraction is 3.5%, and with saturated calomel electrode
It, using 350W xenon lamps as light source, is surveyed on CHI 660D type electrochemical workstations using platinum electrode as auxiliary electrode for reference electrode
Try its photocurrent-time curve.
As seen from Figure 3, when illumination, the density of photocurrent in material increases sharply, and produces a large amount of electronics at this time
And hole, electric current returns near initial value after illumination stops, compared with comparative example 1, comparative example 2 and comparative example 3,1 institute of embodiment
Density of photocurrent of the flower-shaped diamond shape titanium dioxide/graphene composite material of Detitanium-ore-type of preparation under illumination condition obviously carries
Height shows that higher electricity conversion can be obtained in its unique structure.
Claims (5)
1. a kind of preparation side of the flower-shaped diamond shape titanium dioxide/graphene composite material of Detitanium-ore-type for photoproduction cathodic protection
Method, which is characterized in that specifically preparation process is：
(1) titanium tetrachloride solution is added into graphene oxide dispersion, is heated after being sufficiently stirred, heating postcooling to room temperature,
Washing obtains sample drying, is calcined in 400~600 DEG C of nitrogen atmosphere, obtain anatase titanium dioxide crystal seed/stone to neutrality
Black alkene composite material；
(2) titanium tetrachloride solution is added in hydrochloric acid solution and titanium precursors solution is made, step is added into titanium precursors solution
Suddenly the anatase titanium dioxide crystal seed/graphene composite material obtained in (1) obtains mixed dispersion liquid after ultrasonic disperse is uniform,
Mixed dispersion liquid is transferred in water heating kettle, moves to and carries out hydro-thermal reaction in baking oven, reaction postcooling to room temperature filters, and collects
Filter cake is simultaneously washed to neutrality, dry to get to the flower-shaped diamond shape titanium dioxide/graphene photoproduction cathodic protection material of Detitanium-ore-type.
2. compound for the flower-shaped diamond shape titanium dioxide/graphene of Detitanium-ore-type of photoproduction cathodic protection as described in claim 1
The preparation method of material, it is characterised in that：The quality of graphene oxide is dense in graphene oxide dispersion described in step (1)
Degree is 1~2mg/mL；The molar concentration of the titanium tetrachloride solution is 2.5~4.0mol/L；The graphene oxide point
Dispersion liquid and the volume ratio of titanium tetrachloride solution are 45~70:1~2.
3. compound for the flower-shaped diamond shape titanium dioxide/graphene of Detitanium-ore-type of photoproduction cathodic protection as described in claim 1
The preparation method of material, it is characterised in that：Heating temperature described in step (1) is 60~80 DEG C, and heating time is 1~3h；
The drying temperature is 60~80 DEG C；The calcination time is 1~3h.
4. compound for the flower-shaped diamond shape titanium dioxide/graphene of Detitanium-ore-type of photoproduction cathodic protection as described in claim 1
The preparation method of material, it is characterised in that：The molar concentration of titanium tetrachloride solution described in step (2) is 2.5~4.0mol/
L；The molar concentration of the hydrochloric acid solution is 4.0~6.0mol/L.
5. compound for the flower-shaped diamond shape titanium dioxide/graphene of Detitanium-ore-type of photoproduction cathodic protection as described in claim 1
The preparation method of material, it is characterised in that：Hydro-thermal reaction described in step (2) is 150~180 DEG C, and the hydro-thermal reaction time is
10~16h；The drying temperature is 60~80 DEG C.
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| CN112250107A (en) * | 2020-10-21 | 2021-01-22 | 华北电力大学 | Single crystal diamond-shaped titanium dioxide nano-particles and preparation method thereof, and titanium dioxide slurry and application thereof |
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