CN110586930A - Preparation method of nano titanium material for corrosion prevention - Google Patents
Preparation method of nano titanium material for corrosion prevention Download PDFInfo
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- CN110586930A CN110586930A CN201911005768.7A CN201911005768A CN110586930A CN 110586930 A CN110586930 A CN 110586930A CN 201911005768 A CN201911005768 A CN 201911005768A CN 110586930 A CN110586930 A CN 110586930A
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 170
- 239000000463 material Substances 0.000 title claims abstract description 54
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 53
- 239000010936 titanium Substances 0.000 title claims abstract description 53
- 238000005536 corrosion prevention Methods 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000002904 solvent Substances 0.000 claims abstract description 49
- 239000002270 dispersing agent Substances 0.000 claims abstract description 39
- 238000003756 stirring Methods 0.000 claims abstract description 35
- 239000006228 supernatant Substances 0.000 claims abstract description 16
- 238000005119 centrifugation Methods 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 8
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical group CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 15
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 5
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 5
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 5
- 239000001856 Ethyl cellulose Substances 0.000 claims description 4
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 claims description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 4
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 4
- 229920001249 ethyl cellulose Polymers 0.000 claims description 4
- 235000019325 ethyl cellulose Nutrition 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 4
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 3
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 3
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 3
- 239000005642 Oleic acid Substances 0.000 claims description 3
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 3
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 6
- 239000002245 particle Substances 0.000 abstract description 41
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 9
- 229910052744 lithium Inorganic materials 0.000 description 9
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 7
- 229910052782 aluminium Inorganic materials 0.000 description 7
- 238000001878 scanning electron micrograph Methods 0.000 description 7
- 238000001179 sorption measurement Methods 0.000 description 7
- 238000004880 explosion Methods 0.000 description 5
- 230000008595 infiltration Effects 0.000 description 5
- 238000001764 infiltration Methods 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000009826 distribution Methods 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 2
- 230000008676 import Effects 0.000 description 2
- 238000009766 low-temperature sintering Methods 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000011858 nanopowder Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000000527 sonication Methods 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0545—Dispersions or suspensions of nanosized particles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Nanotechnology (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Composite Materials (AREA)
- Materials Engineering (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention relates to a preparation method of a nano titanium material for corrosion prevention, which comprises the following steps of S1: mixing nano titanium powder, a dispersant and a solvent in proportion, stirring by using a stirrer, and then standing; s2: stirring by a stirrer, and then carrying out ultrasonic treatment by ultrasonic waves; s3: centrifuging by using a centrifuge, and taking supernatant liquor after centrifuging; s4: centrifuging the supernatant by using a centrifuge, and taking bottom nano titanium powder after centrifugation; s5: dispersing the bottom layer nano titanium powder in a solvent and stirring by using a stirrer to obtain the nano titanium material for corrosion prevention. According to the preparation method of the nano titanium material for corrosion prevention, provided by the invention, the nano titanium material for corrosion prevention with proper particle size and high concentration is obtained through ultrasonic and centrifugal treatment, and the problems of low purity, overlarge particle size and low apparent density of nano titanium powder in the prior art are solved.
Description
Technical Field
The invention belongs to the technical field of titanium nano materials, and particularly relates to a preparation method of a nano titanium material for corrosion prevention.
Background
The titanium material can be used in an anticorrosive material of a lithium battery aluminum film to improve the overall anticorrosive performance of the material. Especially, when the high-concentration electronic grade nano titanium material is applied to an anticorrosive material of a lithium battery aluminum film, the anticorrosive performance of the nano titanium material is doubled compared with that of a micron-grade titanium material. However, at present, the nano titanium material product is not available in China, and the nano titanium materials required by the aluminum film of the high-end lithium battery are imported.
The preparation difficulty of the nano titanium material is as follows: high-purity nano titanium powder is needed. The nanometer titanium powder has high activity, so that the nanometer titanium powder cannot be produced by a chemical method at present, the nanometer titanium powder prepared by a mechanical ball milling method cannot reach a spherical shape, spherical particles have good filling property and consistency, the nanometer titanium powder prepared by an electric explosion method can reach the shape and the purity, but the particles with the particle size of more than 1 mu m exist, and the nanometer titanium powder cannot be directly applied.
In addition, the loose density of the nano titanium powder is extremely low, so that the nano titanium powder is difficult to achieve high solid content.
Therefore, the development of a preparation method of the nano titanium material for corrosion prevention is a problem to be solved at present.
Disclosure of Invention
Technical problem to be solved
In order to solve the problems in the prior art, the invention provides a preparation method of a nano titanium material for corrosion prevention, which obtains a nano titanium material for corrosion prevention with proper particle size and high concentration through ultrasonic and centrifugal treatment, and solves the problems of low purity, overlarge particle size and low apparent density of nano titanium powder in the prior art.
(II) technical scheme
In order to achieve the purpose, the invention adopts the main technical scheme that:
a preparation method of a nano titanium material for corrosion prevention comprises the following steps,
s1: mixing nano titanium powder, a dispersant and a solvent in proportion, stirring by using a stirrer, and then standing;
s2: stirring by a stirrer, and then carrying out ultrasonic treatment by ultrasonic waves;
s3: centrifuging by using a centrifuge, and taking supernatant liquor after centrifuging;
s4: centrifuging the supernatant by using a centrifuge, and taking bottom nano titanium powder after centrifugation;
s5: dispersing the bottom layer nano titanium powder in a solvent and stirring by using a stirrer to obtain the nano titanium material for corrosion prevention.
Preferably, in the step S1,
the weight ratio of the nano titanium powder to the dispersing agent is 99: 1-85: 15;
the weight ratio of the mixture of the nano titanium powder and the dispersing agent to the solvent is 2: 1-1: 10.
preferably, in the step S1,
the dispersing agent is one or more of polyvinylpyrrolidone, sodium ethyl cellulose, oleic acid, sodium dodecyl benzene sulfonate, polyethylene glycol and polyvinyl alcohol;
the solvent is a volatile solvent, and the solvent is one or more of absolute ethyl alcohol, ethyl acetate and acetone.
Preferably, in the step S1, the stirring time is 1 to 3 hours, and the standing time is 12 to 36 hours.
Preferably, in the step S2, the ultrasonic time is 10-40 minutes, and the ultrasonic temperature does not exceed 40 ℃.
Preferably, in the step S2, the ultrasonic temperature is 10 to 40 ℃.
Preferably, in the step S3, the rotation speed of the centrifuge is 800-.
Preferably, in the step S4, the rotation speed of the centrifuge is 3000-.
Preferably, in the step S5,
the weight ratio of the bottom layer nano titanium powder to the solvent is 0.4: 1-1.5: 1;
the solvent is N-methyl pyrrolidone.
Preferably, in the nano titanium material for corrosion prevention, the average particle size of the nano titanium powder is 70-90 nm.
(III) advantageous effects
The invention has the beneficial effects that:
(1) the problem of large particles in the electric explosion nano titanium powder is solved, and the maximum particles of the nano titanium powder are not more than 1 mu m;
(2) the concentration of the nano titanium powder is more than 50 percent, and the requirement of 25 percent of the concentration of the nano titanium material required by the lithium battery film anticorrosive coating is met and exceeded.
(3) The average particle size of the nano titanium powder prepared by the method is about 80nm, and the used dispersing agent (solvent) has good infiltration and adsorption performance, so that the nano titanium material for corrosion prevention prepared by the method has good stability, and the nano titanium powder is not easy to aggregate and precipitate.
(4) Because the nano titanium powder particles obtained by the preparation method are small, the nano titanium powder can bring better anticorrosion effect when being applied to a lithium battery; meanwhile, the surface of the treated nano titanium powder adsorbs a dispersing agent, the dispersing agent is consistent with a dispersing agent used in an aluminum film anticorrosive coating system of the lithium battery, and in addition, a solvent used in the preparation of the nano titanium material is also consistent with a solvent used in the aluminum film anticorrosive coating system of the lithium battery. Therefore, the nano titanium material has good compatibility with the lithium battery aluminum film anticorrosive coating system.
Drawings
FIG. 1 is a scanning electron microscope image of the nano titanium powder before treatment according to the present invention;
FIG. 2 is a first scanning electron microscope of the treated nano-titanium powder of the present invention;
FIG. 3 is a second scanning electron microscope image of the processed nano-titanium powder of the present invention.
Detailed Description
For a better understanding of the present invention, reference will now be made in detail to the present invention by way of specific embodiments thereof.
The embodiment of the invention discloses a preparation method of a nano titanium material for corrosion prevention, which comprises the following steps,
s1: mixing nano titanium powder, a dispersant and a solvent in proportion, stirring by using a stirrer, and then standing;
s2: stirring by a stirrer, and then carrying out ultrasonic treatment by ultrasonic waves;
s3: centrifuging by using a centrifuge, and taking supernatant liquor after centrifuging;
s4: centrifuging the supernatant by using a centrifuge, and taking bottom nano titanium powder after centrifugation;
s5: dispersing the bottom layer nano titanium powder in a solvent and stirring by using a stirrer to obtain the nano titanium material for corrosion prevention.
The preparation principle of the invention is as follows: after the nano-scale titanium powder is added into the dispersing agent, the nano-scale titanium powder is highly dispersed in an organic solvent, the organic solvent is matched with a lithium battery aluminum film, the product performance can reach the import level, and import substitution is realized.
By the preparation method, in the step S1, the nano titanium powder can be fully dispersed into the solvent under the action of the dispersing agent through mixing and stirring; through standing, the adsorption and infiltration of the dispersing agent on the nano titanium powder can be further promoted and enhanced, so that the stable dispersion of the nano titanium powder in the solvent can be better promoted.
In step S1, after standing, although the adsorption and infiltration of the dispersant to the nano titanium powder are promoted and enhanced, problems such as delamination still occur, and further stirring and ultrasonic treatment are required in step S2 to further promote the adsorption and infiltration of the dispersant to the nano titanium powder.
Preferably, in step S1,
the weight ratio of the nano titanium powder to the dispersing agent is 99: 1-85: 15;
the weight ratio of the mixture of the nano titanium powder and the dispersing agent to the solvent is 2: 1-1: 10.
more preferred ratios are: nano titanium powder: dispersing agent: the solvent is 10:1: 15.
the reason why the above ratio of the titanium powder to the dispersant is preferred is that: the dispersion is not good when the content of the dispersing agent is low, the nano titanium powder is easy to agglomerate, large particles and small particles are difficult to effectively separate, and the net content of the nano titanium powder is reduced when the content of the dispersing agent is too high;
the reason why the above ratio of the mixture of the nano titanium powder and the dispersant to the solvent is preferred is that: if the solvent is too little, the nano titanium powder is difficult to disperse (the concentration is too high), and if the solvent is too much, the concentration of the nano titanium powder is too low, which affects the concentration and the use of the nano titanium material product for corrosion prevention.
Preferably, in step S1,
the dispersant is one or more of polyvinylpyrrolidone, sodium ethyl cellulose, oleic acid, sodium dodecyl benzene sulfonate, polyethylene glycol and polyvinyl alcohol;
the solvent is volatile solvent, and is one or more of absolute ethyl alcohol, ethyl acetate and acetone.
A more preferred dispersant is polyvinylpyrrolidone and a more preferred solvent is absolute ethanol.
The dispersant has the functions of adsorbing the nano titanium powder on the surface and fully dispersing the adsorbed nano titanium powder into the solvent, so that the dispersant can adsorb the nano titanium powder and can also disperse (dissolve) into the solvent through the similarity and intermiscibility principle after adsorption. The dispersant is preferably selected from the group consisting of those having the ability to adsorb the nano-titanium powder and to disperse the nano-titanium powder in the solvent.
The solvent is used for fully dispersing (dissolving) the nano titanium powder adsorbed with the dispersing agent so as to facilitate the treatment of the subsequent centrifugation step.
Preferably, in step S1, the stirring time is 1-3 hours, and the standing time is 12-36 hours.
More preferably, the stirring time is 2 hours and the standing time is 24 hours.
The reason why the above-mentioned time period is preferable for stirring and standing is that: because a lot of gas is adsorbed on the surface of the nano titanium powder, the nano titanium powder and the dispersing agent are added into the solvent together and cannot be immediately soaked, and a certain time is also needed for the dispersing agent to be adsorbed on the surface of the nano titanium powder. The stirring and the standing mainly promote the infiltration of the nano titanium powder and the adsorption of the dispersing agent. If the stirring and standing time is too short, the wetting and adsorption of the dispersing agent and the solvent to the nano titanium powder are insufficient.
Preferably, in step S2, the ultrasonic time is 10-40 minutes, and the ultrasonic temperature is not more than 40 ℃.
More preferably the sonication time is 30 minutes.
The ultrasonic wave is a sound wave with the frequency higher than 20000 Hz, has good directivity and strong penetrating power, is easy to obtain more concentrated sound energy, has long propagation distance in water, and can well disperse or dissolve substances which are difficult to dissolve through high-frequency vibration. In the invention, if the ultrasonic time is short, the nano titanium powder can be agglomerated and cannot be opened, and the small-particle nano titanium powder and the large-particle nano titanium powder cannot be completely separated; the temperature rise can be caused by the overlong ultrasonic time, and the low-temperature sintering of the nano titanium powder can be caused by the temperature rise.
Preferably, in step S2, the ultrasonic temperature is 10-40 ℃.
The reason for controlling the ultrasonic temperature is that an excessively high temperature may cause low-temperature sintering of the nano titanium powder.
Preferably, in step S3, the rotation speed of the centrifuge is 800-1200 rpm, and the centrifugation time is 8-15 minutes.
More preferably, the centrifuge is operated at 1000 rpm for 10 minutes.
The step is the core treatment of the invention, and aims to separate large-particle nano titanium powder from small-particle nano titanium powder, the large-particle nano titanium powder is left on the bottom layer of a centrifugal machine through centrifugation and is separated out, and the supernatant is the target intermediate containing the small-particle nano titanium powder. If the rotating speed of the centrifugal machine is too high and the centrifugal time is too long, a part of small-particle nano titanium powder can be precipitated to the bottom; if the rotating speed of the centrifugal machine is too low or the centrifugal time is too long, the large-particle nano titanium powder can be incompletely removed.
Preferably, in step S4, the rotation speed of the centrifuge is 3000-5000 rpm, and the centrifugation time is 10-40 minutes.
More preferably, the centrifuge is rotated at 4000 rpm for 30 minutes.
The large-particle nano titanium powder is separated by the centrifugal treatment in the first step, and the aim of the step is to prepare the large-particle removed nano titanium powder (highly concentrated nano titanium powder). Therefore, in the centrifugal treatment, when the centrifugal rotating speed of the centrifugal machine is high, the centrifugal is basically not influenced. However, if the centrifugal rotation speed is too low or the centrifugal time is too short, the separation of the nano-powder in the supernatant liquid is not thorough, and the final nano-titanium powder yield is affected.
Preferably, in step S5,
the weight ratio of the bottom layer nano titanium powder to the solvent is 0.4: 1-1.5: 1;
the solvent is N-methyl pyrrolidone.
The more preferable weight ratio of the bottom layer nano titanium powder to the solvent is 1.5: 1.
the comparison between the bottom layer nano titanium powder and the solvent needs to be controlled, and the performance of the final nano titanium material for corrosion prevention is influenced by overhigh or overlow conditions. If the weight ratio of the bottom layer nano titanium powder to the solvent is lower than 0.4: 1, the prepared nano titanium material for corrosion prevention can not meet the requirement of service performance because the content of the nano titanium powder is too low; if the weight ratio of the bottom layer nano titanium powder to the solvent is too high, the viscosity of the nano titanium material system for corrosion prevention is too high, and waste is easily caused in the using process.
In the stirring and dissolution, if the system is free from sludge, it is considered that the stirring is sufficient.
The preferable solvent is N-methyl pyrrolidone, and other similar organic solvents can be used for infiltrating and adsorbing the nano titanium powder, so that the nano titanium powder can be fully dispersed (dissolved) finally.
Preferably, in the nano titanium material for corrosion prevention, the average particle size of the nano titanium powder is 70-90 nm.
More preferably, the average particle size of the nano titanium powder is 80 nm.
The excessive particle size of the nano titanium powder can cause that the high-concentration nano titanium material can not be prepared due to the excessive particle size; if the particle size of the titanium nanopowder is too small, secondary agglomeration will occur due to too high surface activity of the nanoparticles.
The specific process of the method for preparing the nano titanium material for corrosion prevention according to the present invention is exemplified below.
Example 1
S1: mixing nanometer titanium powder (prepared by electric explosion method, purity > 98%, used nanometer titanium powder is particles containing more than 1 um), dispersant polyvinylpyrrolidone (pvp), and anhydrous ethanol according to weight ratio of 10:1:15, stirring with a stirrer for 2 hr, and standing for 24 hr;
s2: fully stirring by using a stirrer, and then carrying out ultrasonic treatment for 30 minutes by using ultrasonic waves, wherein the ultrasonic temperature is not more than 40 ℃;
s3: centrifuging by using a centrifuge at the rotating speed of 1000 revolutions per minute for 10 minutes, and taking supernatant after centrifuging;
s4: centrifuging the supernatant by using a centrifuge at the rotating speed of 4000 revolutions per minute for 30 minutes, and taking bottom-layer nano titanium powder after centrifuging;
s5: dispersing bottom layer nano titanium powder in a solvent N-methyl pyrrolidone (NMP for short) and stirring by a stirrer, wherein the weight ratio of the bottom layer nano titanium powder to the N-methyl pyrrolidone is 1.5: and 1, fully stirring to obtain the nano titanium material for corrosion prevention.
The average grain diameter of the nano titanium powder in the prepared nano titanium material for corrosion prevention is 80 nm.
Example 2
S1: mixing nanometer titanium powder (prepared by electric explosion method, purity > 98%, used nanometer titanium powder is particles containing more than 1 um), dispersant polyvinyl alcohol and acetone according to the weight ratio of 99:1:50, stirring for 3 hours by a stirrer, and then standing for 18 hours;
s2: fully stirring by using a stirrer, and then carrying out ultrasonic treatment for 40 minutes by using ultrasonic waves, wherein the ultrasonic temperature is 30 ℃;
s3: centrifuging by using a centrifuge at the rotating speed of 1200 rpm for 9 minutes, and taking supernatant after centrifuging;
s4: centrifuging the supernatant by using a centrifuge at the rotating speed of 5000 rpm for 15 minutes, and taking bottom-layer nano titanium powder after centrifuging;
s5: dispersing bottom layer nano titanium powder in a solvent N-methyl pyrrolidone (NMP for short) and stirring by a stirrer, wherein the weight ratio of the bottom layer nano titanium powder to the N-methyl pyrrolidone is 0.4: and 1, fully stirring to obtain the nano titanium material for corrosion prevention.
The average particle size of the nano titanium powder in the prepared nano titanium material for corrosion prevention is 90 nm.
Example 3
S1: mixing nano titanium powder (prepared by an electric explosion method, the purity is more than 98 percent, and the used nano titanium powder contains particles with the particle size of more than 1 um), dispersing agents of sodium ethyl cellulose and sodium dodecyl benzene sulfonate, anhydrous ethanol and ethyl acetate according to the weight part ratio of 50:1:500, stirring for 1.5 hours by a stirrer, and then standing for 36 hours;
s2: fully stirring by using a stirrer, and then carrying out ultrasonic treatment for 20 minutes by using ultrasonic waves, wherein the ultrasonic temperature is 20 ℃;
s3: centrifuging by using a centrifuge at the rotating speed of 900 revolutions per minute for 15 minutes, and taking supernatant after centrifuging;
s4: centrifuging the supernatant by using a centrifuge at the rotating speed of 3000 r/min for 40 min, and taking bottom-layer nano titanium powder after centrifuging;
s5: dispersing bottom layer nano titanium powder in a solvent N-methyl pyrrolidone (NMP for short) and stirring by a stirrer, wherein the weight ratio of the bottom layer nano titanium powder to the N-methyl pyrrolidone is 1: and 1, fully stirring to obtain the nano titanium material for corrosion prevention.
The average particle size of the nano titanium powder in the prepared nano titanium material for corrosion prevention is 70 nm.
The nano titanium powder before and after being processed by the preparation method of the invention is tested by a scanning electron microscope (hereinafter referred to as SEM), and the test results are shown in figure 1, figure 2 and figure 3. Wherein:
FIG. 1 is an SEM image of nano titanium powder before being processed by the preparation method of the invention, wherein a scale shown in the SEM image is 1 μm;
FIG. 2 is an SEM image of the nano titanium powder treated by the preparation method of the present invention, wherein the scale shown in the SEM image is 1 μm;
FIG. 3 is an SEM image of the nano titanium powder treated by the preparation method of the present invention, wherein the scale shown in the SEM image is 300 nm.
By comparing with fig. 1 and fig. 2, the size distribution of the nano titanium powder before treatment in fig. 1 is wide, and the size particles are all present; after the nano titanium powder is treated by the preparation method, the nano titanium powder treated in the figure 2 has uniform size distribution, uniform particle size and no large particles.
And when being compared with the figures 2 and 3, the two figures are SEM images of the nano titanium powder treated by the method. Under the scale of 300nm, no obvious large particles are seen when the nano titanium powder particles are seen in an enlarged manner, which shows that the nano titanium powder treated by the preparation method has more uniform particle size, narrower particle size distribution and more stable product performance.
Finally, it should be noted that: the above-mentioned embodiments are only used for illustrating the technical solution of the present invention, and not for limiting the same; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. A preparation method of a nano titanium material for corrosion prevention is characterized by comprising the following steps: comprises the following steps of (a) carrying out,
s1: mixing nano titanium powder, a dispersant and a solvent in proportion, stirring by using a stirrer, and then standing;
s2: stirring by a stirrer, and then carrying out ultrasonic treatment by ultrasonic waves;
s3: centrifuging by using a centrifuge, and taking supernatant liquor after centrifuging;
s4: centrifuging the supernatant by using a centrifuge, and taking bottom nano titanium powder after centrifugation;
s5: dispersing the bottom layer nano titanium powder in a solvent and stirring by using a stirrer to obtain the nano titanium material for corrosion prevention.
2. The method for preparing the nano titanium material for corrosion prevention according to claim 1, characterized in that:
in the step S1, in the above step,
the weight ratio of the nano titanium powder to the dispersing agent is 99: 1-85: 15;
the weight ratio of the mixture of the nano titanium powder and the dispersing agent to the solvent is 2: 1-1: 10.
3. the method for preparing the nano titanium material for corrosion prevention according to claim 1, characterized in that:
in the step S1, in the above step,
the dispersing agent is one or more of polyvinylpyrrolidone, sodium ethyl cellulose, oleic acid, sodium dodecyl benzene sulfonate, polyethylene glycol and polyvinyl alcohol;
the solvent is a volatile solvent, and the solvent is one or more of absolute ethyl alcohol, ethyl acetate and acetone.
4. The method for producing a nano titanium material for corrosion prevention according to any one of claims 1 to 3, characterized in that:
in the step S1, the stirring time is 1-3 hours, and the standing time is 12-36 hours.
5. The method for producing a nano titanium material for corrosion prevention according to claim 1 or 2, characterized in that: in the step S2, the ultrasonic time is 10-40 minutes, and the ultrasonic temperature is not more than 40 ℃.
6. The method for preparing a nano titanium material for corrosion prevention according to claim 5, characterized in that: in the step S2, the ultrasonic temperature is 10-40 ℃.
7. The method for producing a nano titanium material for corrosion prevention according to claim 1 or 2, characterized in that: in step S3, the rotation speed of the centrifuge is 800-1200 rpm, and the centrifugation time is 8-15 minutes.
8. The method for producing a nano titanium material for corrosion prevention according to claim 1 or 2, characterized in that: in step S4, the rotation speed of the centrifuge is 3000-5000 rpm, and the centrifugation time is 10-40 minutes.
9. The method for producing a nano titanium material for corrosion prevention according to claim 1 or 2, characterized in that: in the step S5, the ratio of the bottom layer nano titanium powder to the solvent in parts by weight is 0.4: 1-1.5: 1;
the solvent is N-methyl pyrrolidone.
10. The method for producing a nano titanium material for corrosion prevention according to claim 1 or 2, characterized in that: in the nano titanium material for corrosion prevention, the average grain diameter of nano titanium powder is 70-90 nm.
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Denomination of invention: A preparation method of nano titanium materials for corrosion prevention Granted publication date: 20220114 Pledgee: Guangdong Shunde Rural Commercial Bank Co.,Ltd. science and technology innovation sub branch Pledgor: GUANGDONG YINNA TECHNOLOGY CO.,LTD. Registration number: Y2024980013051 |