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CN113681018A - Preparation method of ultrathin porous micron zinc sheet - Google Patents

Preparation method of ultrathin porous micron zinc sheet Download PDF

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Publication number
CN113681018A
CN113681018A CN202111010283.4A CN202111010283A CN113681018A CN 113681018 A CN113681018 A CN 113681018A CN 202111010283 A CN202111010283 A CN 202111010283A CN 113681018 A CN113681018 A CN 113681018A
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zinc
ultra
thin porous
preparing
inert gas
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Inventor
唐少春
吴懿鹏
张青原
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HAIAN INSTITUTE OF HIGH-TECH RESEARCH NANJING UNIVERSITY
Nanjing University
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HAIAN INSTITUTE OF HIGH-TECH RESEARCH NANJING UNIVERSITY
Nanjing University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/12Making metallic powder or suspensions thereof using physical processes starting from gaseous material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/043Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling

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Abstract

The invention discloses a preparation method of an ultrathin porous micron zinc sheet. The zinc sheet is in the form of scale powder and has the characteristics of large diameter-thickness ratio and ultra-thin. Firstly, heating and melting a high-purity zinc ingot in a melting and liquating furnace, converting the high-purity zinc ingot into steam, introducing the zinc steam into a condenser filled with inert gas, and attracting submicron or nanometer zinc powder particles in the condenser and aerosol formed by the inert gas into a condensation cyclone separator through an exhaust fan under the protection of the inert gas to obtain submicron spherical zinc powder. Then, the spherical zinc powder with submicron scale is subjected to ball milling, centrifugal separation and vacuum drying to obtain the ultrathin porous zinc micron sheet.

Description

Preparation method of ultrathin porous micron zinc sheet
Technical Field
The invention relates to the field of preparation of ultrathin porous micron zinc sheets.
Background
The ultrathin porous micron zinc sheet is an important raw material for producing water-soluble inorganic salt paint, inorganic zinc-rich paint and dacromet coating liquid, and has incomparable advantages compared with other micron/nanometer inorganic powder materials in the field of metal deep corrosion prevention. The production method commonly used at present comprises an explosion method, a ball milling method, an electrolysis method and the like, but the product has the defects of high oxidation rate, low purity, uneven particle size distribution, narrow extension plane range, low diameter-thickness ratio, low flaking rate and the like.
Disclosure of Invention
The invention overcomes the defects and provides a preparation method of an ultrathin porous micron zinc sheet, which is characterized by comprising the following steps:
A. heating and melting a high-purity zinc ingot in a melting and liquating furnace, and converting the high-purity zinc ingot into steam;
B. introducing the vapor obtained in the step A into a condenser filled with inert gas, and under the protection of the inert gas, sucking aerosol formed by submicron or nanometer zinc powder particles and the inert gas in the condenser into a condensation cyclone separator by an exhaust fan to obtain submicron spherical zinc powder;
C. b, ball milling the spherical zinc powder obtained in the step B together with solvent oil and an auxiliary agent;
D. c, performing centrifugal treatment on the zinc powder subjected to ball milling treatment obtained in the step C;
E. and D, placing the zinc powder obtained in the step D into a vacuum drying furnace, drying at a certain temperature, and cooling to room temperature along with the furnace to obtain the ultrathin porous zinc micron sheet.
The preparation method of the ultrathin porous micron zinc sheet is further improved in that the zinc content of the high-purity zinc ingot is more than or equal to 99.99%.
The preparation method of the ultrathin porous micron zinc sheet is further improved in that the high-purity zinc ingot is heated and melted in a melting and liquating furnace at the temperature of 950-1100 ℃.
The preparation method of the ultrathin porous micron zinc sheet is further improved in that the inert gas is argon.
The preparation method of the ultrathin porous micron zinc sheet is further improved in that the rotating speed of the ball milling ball mill is 500-800 r/min.
The preparation method of the ultrathin porous micron zinc sheet is further improved in that the ball milling treatment time is 1-2 hours.
The preparation method of the ultrathin porous micron zinc sheet is further improved in that the centrifugal treatment time is 3-4 hours.
The preparation method of the ultrathin porous micron zinc sheet is further improved in that the vacuum drying air pressure is 0.5-2 Pa.
The preparation method of the ultrathin porous micron zinc sheet is further improved in that the vacuum drying temperature is 200-400 ℃.
The preparation method of the ultrathin porous micron zinc sheet is further improved in that the vacuum drying treatment time is more than 6 hours.
The ultrathin porous micron zinc sheet prepared by the method has the characteristics of large diameter-thickness ratio and ultrathin property, has obvious corrosion prevention and oxidation resistance effects, high activity and excellent conductivity, realizes high efficiency, short period, low energy consumption and zero emission, and meets the application requirements of different fields.
Drawings
FIG. 1 is an SEM photograph of a zinc sheet prepared by the preparation method of the ultrathin porous micron zinc sheet.
Detailed Description
The present invention will be further illustrated with reference to the following specific examples, but the present invention is not limited to the following examples.
Example 1:
heating a high-purity zinc ingot with the zinc content of more than or equal to 99.99 percent to 950 ℃ in a melting and liquating furnace for melting and converting into steam; introducing steam into a condenser filled with argon, and under the protection of inert gas argon, sucking aerosol formed by submicron or nanometer zinc powder particles and inert gas in the condenser into a condensation cyclone separator through an exhaust fan to obtain submicron spherical zinc powder; carrying out ball milling treatment on the obtained spherical zinc powder, solvent oil and an auxiliary agent together, wherein the rotating speed of a ball mill is 500 r/min, and the ball milling treatment time is 2 hours; carrying out centrifugal treatment on the obtained zinc powder subjected to ball milling treatment for 4 hours; then placing the mixture in a vacuum drying furnace with the air pressure of 0.5Pa, drying the mixture for more than 6 hours at the temperature of 400 ℃, and cooling the mixture to room temperature along with the furnace to obtain the ultrathin porous zinc micron sheet.
Example 2:
heating a high-purity zinc ingot with the zinc content of more than or equal to 99.99 percent to 1000 ℃ in a melting and liquating furnace for melting and converting into steam; introducing steam into a condenser filled with argon, and under the protection of inert gas argon, sucking aerosol formed by submicron or nanometer zinc powder particles and inert gas in the condenser into a condensation cyclone separator through an exhaust fan to obtain submicron spherical zinc powder; carrying out ball milling treatment on the obtained spherical zinc powder, solvent oil and an auxiliary agent together, wherein the rotating speed of a ball mill is 600 revolutions per minute, and the ball milling treatment time is 1.5 hours; carrying out centrifugal treatment on the obtained zinc powder subjected to ball milling treatment for 4 hours; and then placing the mixture in a vacuum drying furnace with the air pressure of 1Pa, drying the mixture for more than 6 hours at the temperature of 300 ℃, and cooling the mixture to room temperature along with the furnace to obtain the ultrathin porous zinc micron sheet.
Example 3:
heating a high-purity zinc ingot with the zinc content of more than or equal to 99.99 percent to 1100 ℃ in a melting and liquating furnace for melting and converting into steam; introducing steam into a condenser filled with argon, and under the protection of inert gas argon, sucking aerosol formed by submicron or nanometer zinc powder particles and inert gas in the condenser into a condensation cyclone separator through an exhaust fan to obtain submicron spherical zinc powder; carrying out ball milling treatment on the obtained spherical zinc powder, solvent oil and an auxiliary agent together, wherein the rotating speed of a ball mill is 700 r/min, and the ball milling treatment time is 1 hour; carrying out centrifugal treatment on the obtained zinc powder subjected to ball milling treatment for 3 hours; then placing the mixture in a vacuum drying furnace with the air pressure of 1.5Pa, drying the mixture for more than 6 hours at the temperature of 200 ℃, and cooling the mixture to room temperature along with the furnace to obtain the ultrathin porous zinc micron sheet.
Example 4:
heating a high-purity zinc ingot with the zinc content of more than or equal to 99.99 percent to 1100 ℃ in a melting and liquating furnace for melting and converting into steam; introducing steam into a condenser filled with argon, and under the protection of inert gas argon, sucking aerosol formed by submicron or nanometer zinc powder particles and inert gas in the condenser into a condensation cyclone separator through an exhaust fan to obtain submicron spherical zinc powder; carrying out ball milling treatment on the obtained spherical zinc powder, solvent oil and an auxiliary agent together, wherein the rotating speed of a ball mill is 800 r/min, and the ball milling treatment time is 1 hour; carrying out centrifugal treatment on the obtained zinc powder subjected to ball milling treatment for 3 hours; and then placing the mixture in a vacuum drying furnace with the air pressure of 2Pa, drying the mixture for more than 6 hours at the temperature of 250 ℃, and cooling the mixture to room temperature along with the furnace to obtain the ultrathin porous zinc micron sheet.
The ultrathin porous micron zinc sheet prepared by the invention has uniform particle size distribution and low thickness, and the particle size and thickness are tested as follows:
Figure 358822DEST_PATH_IMAGE001
finally, it should be noted that although the above embodiments have been described herein, the scope of the present invention is not limited thereby. Therefore, based on the innovative concepts of the present invention, the technical solutions of the present invention can be directly or indirectly applied to other related technical fields by making changes and modifications to the embodiments described herein or by using equivalent structures or equivalent processes performed in the specification and the drawings of the present invention, and are included in the scope of the present invention.

Claims (10)

1.一种超薄多孔微米锌片的制备方法,其特征在于:步骤如下:1. a preparation method of ultra-thin porous micron zinc sheet, is characterized in that: step is as follows: A、将高纯锌锭在熔化熔析炉中加热熔化,并转化为蒸气;A. The high-purity zinc ingot is heated and melted in the melting furnace and converted into steam; B、将步骤A得到的蒸气引入充满惰性气体的冷凝器中,在惰性气体保护下通过抽风机将冷凝器中的亚微米级或纳米级锌粉颗粒以及惰性气体形成的气溶胶吸引到冷凝旋风分离器中得到亚微米球形锌粉;B. The vapor obtained in step A is introduced into a condenser filled with inert gas, and the aerosol formed by the submicron-scale or nano-scale zinc powder particles and the inert gas in the condenser is attracted to the condensation cyclone by the suction fan under the protection of the inert gas Submicron spherical zinc powder is obtained in the separator; C、将步骤B得到的球形锌粉与溶剂油及助剂一同进行球磨处理;C, the spherical zinc powder that step B obtains is carried out ball milling together with solvent oil and auxiliary agent; D、将步骤C得到的球磨处理后的锌粉进行离心处理;D, the zinc powder after the ball milling treatment that step C obtains is carried out centrifugal treatment; E、将步骤D得到的锌粉置于真空干燥炉内,一定温度下进行干燥处理,并随炉冷却至室温,得到超薄多孔锌微米片。E. The zinc powder obtained in step D is placed in a vacuum drying furnace, dried at a certain temperature, and cooled to room temperature with the furnace to obtain ultra-thin porous zinc micro-flakes. 2.根据权利要求1所述的一种超薄多孔微米锌片的制备方法,其特征在于:所述高纯锌锭含锌量≥99.99%。2 . The method for preparing an ultra-thin porous micron zinc flake according to claim 1 , wherein the zinc content of the high-purity zinc ingot is greater than or equal to 99.99%. 3 . 3.根据权利要求2所述的一种超薄多孔微米锌片的制备方法,其特征在于:所述高纯锌锭在熔化熔析炉中加热熔化温度为950~1100℃。3 . The method for preparing an ultra-thin porous micro-zinc sheet according to claim 2 , wherein the high-purity zinc ingot is heated and melted at a temperature of 950-1100° C. in a melting and melting furnace. 4 . 4.根据权利要求1所述的一种超薄多孔微米锌片的制备方法,其特征在于:所述惰性气体为氩气。4 . The method for preparing an ultra-thin porous micro-zinc sheet according to claim 1 , wherein the inert gas is argon. 5 . 5.根据权利要求1所述的一种超薄多孔微米锌片的制备方法,其特征在于:所述球磨处理球磨机转速为500-800转/分钟。5 . The method for preparing an ultra-thin porous micro-zinc sheet according to claim 1 , wherein the rotating speed of the ball mill for ball milling is 500-800 rpm. 6 . 6.根据权利要求1所述的一种超薄多孔微米锌片的制备方法,其特征在于:所述球磨处理时间为1~2小时。6 . The method for preparing an ultra-thin porous micron zinc flake according to claim 1 , wherein the ball milling treatment time is 1 to 2 hours. 7 . 7.根据权利要求1所述的一种超薄多孔微米锌片的制备方法,其特征在于:所述离心处理时间为3~4小时。7. the preparation method of a kind of ultra-thin porous micron zinc flake according to claim 1, is characterized in that: described centrifugal treatment time is 3~4 hours. 8.根据权利要求1所述的一种超薄多孔微米锌片的制备方法,其特征在于:所述真空干燥气压为0.5~2Pa。8 . The method for preparing an ultra-thin porous micro-zinc sheet according to claim 1 , wherein the vacuum drying air pressure is 0.5 to 2 Pa. 9 . 9.根据权利要求8所述的一种超薄多孔微米锌片的制备方法,其特征在于:所述真空干燥温度为200~400℃。9 . The method for preparing an ultra-thin porous micro-zinc sheet according to claim 8 , wherein the vacuum drying temperature is 200-400° C. 10 . 10.根据权利要求9所述的一种超薄多孔微米锌片的制备方法,其特征在于:所述真空干燥处理时间为6小时以上。10 . The method for preparing an ultra-thin porous micron zinc flake according to claim 9 , wherein the vacuum drying treatment time is more than 6 hours. 11 .
CN202111010283.4A 2021-08-31 2021-08-31 Preparation method of ultrathin porous micron zinc sheet Pending CN113681018A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1431074A (en) * 2003-01-24 2003-07-23 翟国华 Method for producing zinc powder and its mfg. device
US20050150984A1 (en) * 2002-09-23 2005-07-14 Savin Ronald R. Process for dry milling zinc powder to produce zinc flake
CN101391305A (en) * 2008-11-04 2009-03-25 昆明海创兴科技有限公司 Manufacture method of superfine laminar zinc powder and zinc pulp
CN101618458A (en) * 2009-07-17 2010-01-06 江苏科创金属新材料有限公司 Preparation method of sub-micron zinc powder and preparation device thereof
CN104815987A (en) * 2015-05-07 2015-08-05 昆明冶金研究院 Flaky zinc powder preparation method
CN112846207A (en) * 2021-01-15 2021-05-28 昆明冶金研究院有限公司 Preparation method of superfine active zinc powder

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20050150984A1 (en) * 2002-09-23 2005-07-14 Savin Ronald R. Process for dry milling zinc powder to produce zinc flake
CN1431074A (en) * 2003-01-24 2003-07-23 翟国华 Method for producing zinc powder and its mfg. device
CN101391305A (en) * 2008-11-04 2009-03-25 昆明海创兴科技有限公司 Manufacture method of superfine laminar zinc powder and zinc pulp
CN101618458A (en) * 2009-07-17 2010-01-06 江苏科创金属新材料有限公司 Preparation method of sub-micron zinc powder and preparation device thereof
CN104815987A (en) * 2015-05-07 2015-08-05 昆明冶金研究院 Flaky zinc powder preparation method
CN112846207A (en) * 2021-01-15 2021-05-28 昆明冶金研究院有限公司 Preparation method of superfine active zinc powder

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
严海锦等: "超薄超细鳞片状锌粉(锌片)制备技术研究", 《上海化工》 *

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