CN114042920A - Superfine flaky zinc powder and preparation process thereof - Google Patents

Superfine flaky zinc powder and preparation process thereof Download PDF

Info

Publication number
CN114042920A
CN114042920A CN202111352529.6A CN202111352529A CN114042920A CN 114042920 A CN114042920 A CN 114042920A CN 202111352529 A CN202111352529 A CN 202111352529A CN 114042920 A CN114042920 A CN 114042920A
Authority
CN
China
Prior art keywords
zinc powder
ball
ball milling
milling
flaky zinc
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202111352529.6A
Other languages
Chinese (zh)
Inventor
白江博
刘忠庆
程乐心
郑桃
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Suzhou Wave Vector New Material Technology Co ltd
Original Assignee
Suzhou Wave Vector New Material Technology Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Suzhou Wave Vector New Material Technology Co ltd filed Critical Suzhou Wave Vector New Material Technology Co ltd
Priority to CN202111352529.6A priority Critical patent/CN114042920A/en
Publication of CN114042920A publication Critical patent/CN114042920A/en
Pending legal-status Critical Current

Links

Classifications

    • 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
    • B22F2009/042Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling using a particular milling fluid
    • 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

Landscapes

  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention belongs to the technical field of manufacturing of flake zinc powder, and particularly relates to superfine flake zinc powder and a preparation process thereof. Adding medium balls, ball-milling solution and zinc powder raw materials into a ball-milling device for ball-milling, separating out solids after ball-milling, and drying and grading to obtain superfine flaky zinc powder; wherein the ball milling solution is a mixed solution of deionized water and DMAC. The process provided by the invention can safely and stably produce the flaky zinc powder with uniform, high zinc content and good glossiness in an industrialized way. Compared with dry ball milling, the process of the invention does not need inert gas protection, reduces the requirements on equipment and production cost, and effectively reduces powder agglomeration and welding. Compared with wet ball milling with organic solvent, the process of the invention solves the problems of flammable and explosive hidden troubles caused by volatilization of the organic solvent and harm to human bodies and environment. Compared with the deionized water wet ball milling, the process slows down the oxidation process of the zinc powder in the ball milling process, and improves the zinc content and the brightness of the flaky zinc powder.

Description

Superfine flaky zinc powder and preparation process thereof
Technical Field
The invention belongs to the technical field of manufacturing of flake zinc powder, and particularly relates to superfine flake zinc powder and a preparation process thereof.
Background
Dacromet is a zinc-based water-based corrosion-resistant coating technology, which is mainly applied to the surface treatment of steel, and is prepared by coating or dipping a metal matrix with a treatment solution prepared from substances including flaky zinc powder, a corrosion inhibitor and the like, and forming a firm compact corrosion-resistant coating on the surface of the matrix metal after baking. The Dacromet coating has the triple functions of shielding, cathode protection and corrosion inhibition, has good corrosion resistance, low cost, less environmental pollution than electrogalvanizing, wide application prospect and higher economic value.
Flaky zinc powder is an important raw material in a dacromet coating and needs to meet very strict requirements. The flaky zinc powder is required to have large hiding power and floatability, and to have good dispersibility and brightness.
At present, the preparation method of the superfine flaky zinc powder is mainly divided into a wet method and a dry method. For example, patent CN103341632A provides a dry ball milling process, in which zinc powder and a ball milling medium are ball milled and sieved in a closed roller ball mill under the protection of inert gas and the action of a composite assistant to obtain flake zinc powder; for another example, patent CN110405199A provides a wet ball milling process, which is carried out by twice milling under the conditions of organic solvent and grinding aid and cyclone separation to obtain flaky zinc powder.
However, the existing dry process and wet process still have some technical defects which are difficult to overcome respectively.
1) And (3) dry ball milling process. The dry production process has short flow, but the equipment is complicated, inert gas protection is usually needed, and the prepared flaky zinc powder has poor uniformity and high zinc oxide content. In addition, zinc is a metal with excellent ductility, and adheres to the surface of the polishing medium during polishing, thereby reducing the polishing efficiency. When the size of the zinc powder is small to a certain degree, the surface energy is increased sharply, the crushing resistance caused by the surface energy is difficult to overcome only by mechanical force, and the prepared zinc powder is agglomerated and welded due to the overhigh surface energy.
2) Wet ball milling using an organic solvent. Grinding aids such as mineral spirits, glycols, etc. are used to provide dispersing, grinding aid and anti-oxidation. The addition of the grinding aid such as the solvent oil can enable the flaky zinc powder to meet the requirements, but has the problems of flammability, explosiveness, high toxicity and the like, is difficult to store, is harmful to the environment and the bodies of workers, cannot meet the requirements of environmental protection and fire safety, and is difficult to realize large-scale industrial production.
3) And ball milling by using a deionized water wet method. Although deionized water has a good grinding-aiding effect, the flaky zinc powder prepared by the deionized water has low metal zinc content and cannot meet the use requirement. The lower content of metal zinc is because zinc powder reacts with oxygen, carbon dioxide and the like in deionized water to generate basic zinc carbonate, and the reaction formula is 4Zn +2O2+CO2+3H2O=ZnCO3•3Zn(OH)2. Meanwhile, the existence of the basic zinc carbonate also shortens the service life of the steel ball.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides superfine flaky zinc powder and a preparation process thereof. The novel preparation process provided by the invention aims to solve and improve various technical defects of the existing process, and specifically comprises the following steps: the flaky zinc powder with uniform, high zinc content and good glossiness is safely and stably produced in an industrialized way; inert gas protection is not used, so that the requirement on equipment is lowered; inhibiting the agglomeration and welding of zinc powder; solves the problems of flammability, explosiveness, health damage and the like caused by organic solvents.
In order to achieve the above object, the present invention is achieved by the following technical means. A preparation process of superfine flaky zinc powder comprises the steps of adding medium balls, a ball-milling solution and a zinc powder raw material into a ball-milling device for ball milling, separating out solids after ball milling, drying and grading to obtain the superfine flaky zinc powder with the particle size of 15-25 mu m of D50; the ball milling solution is a mixed solution of deionized water and DMAC, and the mass ratio of the DMAC to the water is controlled to be 3-8: 1.
Further, the medium ball is a stainless steel ball; the diameter of the stainless steel ball is controlled to be 1.5-5 mm; controlling the ball-material ratio to be 3-10: 1; the liquid-material ratio is controlled to be 2-5: 1.
The ball-material ratio is too small, the ball milling efficiency is reduced, the milling time is prolonged, and the oxidation of zinc powder is aggravated; the ball-material ratio is too large, so that the ball milling efficiency can be improved, but the particle size of the prepared flaky zinc powder is small, and the flake thickness ratio is small.
The diameter of the medium ball is too small, the number of the medium balls is increased, the contact area with the material is increased, the friction surface is increased, the grinding effect is good, but the mass of the medium ball is correspondingly small, the impact shearing effect of the medium ball is not obvious, and the grinding time is long; the diameter of the medium ball is too large, so that the grinding time is shortened, but the impact shearing action is too strong, so that the prepared flaky zinc powder has non-uniform particle size and larger difference.
The liquid-material ratio is larger, the ball milling efficiency is reduced, the particle size of the flaky powder is larger, and the yield is low; the liquid-material ratio is smaller, the ball milling slurry has poor fluidity, the ball milling effect is not uniform, and the thickness deviation of the flaky zinc powder is large.
Further optimizing, and controlling the diameter of the stainless steel ball to be 2-3 mm; controlling the ball-material ratio to be 5-8: 1; the liquid-material ratio is controlled to be 3-4: 1.
Further, if the proportion of DMAC and water is larger, the ball milling efficiency is reduced; if the proportion is smaller, the powder is more oxidized. More preferably, the mass ratio of DMAC to water is controlled to be 4-6: 1.
Further, the ball milling speed is controlled to be 200-500 r/min, and the ball milling time is controlled to be 3-6 h.
Further, the apparent density of the prepared superfine flaky zinc powder is controlled to be 0.5-1.0 g/cm3
And further, after the ball milling is finished, carrying out filter pressing on the slurry obtained by the ball milling to separate out a solid, and then transferring the solid to a vacuum drying oven for drying.
Further, the drying temperature is set to be 100-150 ℃, and the drying time is 2-6 h.
Has the advantages that:
the superfine flaky zinc powder ball milling process provided by the invention can safely and stably produce flaky zinc powder with uniform zinc content and good glossiness in an industrialized way. Compared with dry ball milling, the process of the invention does not need inert gas protection, reduces the requirements on equipment and production cost, and effectively reduces powder agglomeration and welding. Compared with wet ball milling with organic solvent, the process of the invention solves the problems of flammable and explosive hidden troubles caused by volatilization of the organic solvent and harm to human bodies and environment. Compared with the deionized water wet ball milling, the process slows down the oxidation process of the zinc powder in the ball milling process, and improves the zinc content and the brightness of the flaky zinc powder.
Detailed Description
The invention is further illustrated by the following specific examples, which are illustrative and intended to illustrate the problem and explain the invention, but not limiting.
Example 1
Adding medium balls, ball-milling solution and zinc powder raw materials into a ball-milling device for ball milling, after the ball milling is finished, carrying out filter pressing on slurry obtained by the ball milling to separate out solids, then transferring the solids to a vacuum drying oven for drying, and finally grading to obtain the superfine flaky zinc powder.
In this embodiment, the ball-milling solution is a uniformly mixed solution obtained by stirring deionized water and DMAC at a low speed for 0.5h, and the mass ratio of DMAC to water is 3: 1.
In this embodiment, the medium ball is a stainless steel ball; the diameter of the stainless steel ball is 1.5 mm; the ball material ratio is 3: 1; the liquid-material ratio is 5: 1.
In this example, the ball milling speed was 500r/min, and the ball milling time was 6 hours.
In this example, the drying temperature was 100 ℃ and the drying time was 6 hours.
In this example, an ultrafine flaky zinc powder having a D50 value of 23.3 μm and a loose density of 0.68g/cm was obtained by classification3
Example 2
Adding medium balls, ball-milling solution and zinc powder raw materials into a ball-milling device for ball milling, after the ball milling is finished, carrying out filter pressing on slurry obtained by the ball milling to separate out solids, then transferring the solids to a vacuum drying oven for drying, and finally grading to obtain the superfine flaky zinc powder.
In this embodiment, the ball-milling solution is a uniformly mixed solution obtained by stirring deionized water and DMAC at a low speed for 0.5h, and the mass ratio of DMAC to water is 4: 1.
In this embodiment, the medium ball is a stainless steel ball; the diameter of the stainless steel ball is 2 mm; the ball material ratio is 5: 1; the liquid-material ratio is 4: 1.
In this example, the ball milling speed was 400r/min, and the ball milling time was 5 hours.
In this example, the drying temperature was 110 ℃ and the drying time was 5 hours.
In this example, an ultrafine flaky zinc powder having a D50 value of 20.4 μm and a loose density of 0.76g/cm was obtained by classification3
Example 3
Adding medium balls, ball-milling solution and zinc powder raw materials into a ball-milling device for ball milling, after the ball milling is finished, carrying out filter pressing on slurry obtained by the ball milling to separate out solids, then transferring the solids to a vacuum drying oven for drying, and finally grading to obtain the superfine flaky zinc powder.
In this embodiment, the ball-milling solution is a uniformly mixed solution obtained by stirring deionized water and DMAC at a low speed for 0.5h, and the mass ratio of DMAC to water is 6: 1.
In this embodiment, the medium ball is a stainless steel ball; the diameter of the stainless steel ball is 3 mm; the ball material ratio is 8: 1; the liquid-material ratio is 3: 1.
In this example, the ball milling speed was 300r/min, and the ball milling time was 4 hours.
In this example, the drying temperature was 130 ℃ and the drying time was 4 hours.
In this example, an ultrafine flaky zinc powder having a D50 value of 19.0 μm and a loose density of 0.89g/cm was obtained by classification3
Example 4
Adding medium balls, ball-milling solution and zinc powder raw materials into a ball-milling device for ball milling, after the ball milling is finished, carrying out filter pressing on slurry obtained by the ball milling to separate out solids, then transferring the solids to a vacuum drying oven for drying, and finally grading to obtain the superfine flaky zinc powder.
In this embodiment, the ball-milling solution is a uniformly mixed solution obtained by stirring deionized water and DMAC at a low speed for 0.5h, and the mass ratio of DMAC to water is 8: 1.
In this embodiment, the medium ball is a stainless steel ball; the diameter of the stainless steel ball is 5 mm; the ball material ratio is 10: 1; the liquid-material ratio is 2: 1.
In this example, the ball milling speed was 200r/min, and the ball milling time was 3 hours.
In this example, the drying temperature was 150 ℃ and the drying time was 2 hours.
In this example, an ultrafine flaky zinc powder having a D50 value of 17.9 μm and a loose density of 0.96g/cm was obtained by classification3
The above embodiments are exemplary only, and are intended to illustrate the technical concept and features of the present invention so that those skilled in the art can understand the contents of the present invention and implement the present invention, and not to limit the scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.

Claims (9)

1. A preparation process of superfine flaky zinc powder is characterized by comprising the following steps: adding medium balls, a ball milling solution and zinc powder raw materials into a ball milling device for ball milling, separating out solids after the ball milling is finished, and drying and grading to obtain superfine flaky zinc powder with the particle size of D50 being 15-25 mu m; the ball milling solution is a mixed solution of deionized water and DMAC, and the mass ratio of the DMAC to the water is controlled to be 3-8: 1.
2. The process for preparing ultrafine flaky zinc powder according to claim 1, characterized in that: the medium ball is a stainless steel ball; the diameter of the stainless steel ball is controlled to be 1.5-5 mm; controlling the ball-material ratio to be 3-10: 1; the liquid-material ratio is controlled to be 2-5: 1.
3. The process for preparing ultrafine flaky zinc powder according to claim 2, characterized in that: the diameter of the stainless steel ball is controlled to be 2-3 mm; controlling the ball-material ratio to be 5-8: 1; the liquid-material ratio is controlled to be 3-4: 1.
4. The process for preparing ultrafine flaky zinc powder according to claim 1, characterized in that: the mass ratio of DMAC and water is controlled to be 4-6: 1.
5. The process for preparing ultrafine flaky zinc powder according to claim 1, characterized in that: the ball milling speed is 200-500 r/min, and the ball milling time is 3-6 h.
6. The process for preparing ultrafine flaky zinc powder according to claim 1, characterized in that: the apparent density of the prepared superfine flaky zinc powder is controlled to be 0.5-1.0 g/cm3
7. The process for preparing ultrafine flaky zinc powder according to claim 1, characterized in that: and after the ball milling is finished, carrying out filter pressing on the slurry obtained by the ball milling to separate out a solid, and then transferring the solid to a vacuum drying oven for drying.
8. The process for preparing ultrafine flaky zinc powder according to claim 7, which is characterized in that: the drying temperature is 100 ℃ and 150 ℃, and the drying time is 2-6 h.
9. An ultrafine flaky zinc powder is characterized in that: the ultra-fine flaky zinc powder as defined in any one of claims 1 to 8.
CN202111352529.6A 2021-11-16 2021-11-16 Superfine flaky zinc powder and preparation process thereof Pending CN114042920A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202111352529.6A CN114042920A (en) 2021-11-16 2021-11-16 Superfine flaky zinc powder and preparation process thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202111352529.6A CN114042920A (en) 2021-11-16 2021-11-16 Superfine flaky zinc powder and preparation process thereof

Publications (1)

Publication Number Publication Date
CN114042920A true CN114042920A (en) 2022-02-15

Family

ID=80209087

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202111352529.6A Pending CN114042920A (en) 2021-11-16 2021-11-16 Superfine flaky zinc powder and preparation process thereof

Country Status (1)

Country Link
CN (1) CN114042920A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115650196A (en) * 2022-09-09 2023-01-31 株洲冶炼集团股份有限公司 Synthesis method of zinc metaphosphate and application of zinc metaphosphate in thallium removal of zinc sulfate solution

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102248176A (en) * 2011-07-15 2011-11-23 云南铜业科技发展股份有限公司 Preparation method of flake silver powder with low burning loss
CN102392254A (en) * 2011-10-31 2012-03-28 西安理工大学 Water-soluble corrosion inhibitor and method for preparing zinc slurry by using the same
CN103204525A (en) * 2012-01-17 2013-07-17 上海杰事杰新材料(集团)股份有限公司 Application of lactam as solvent in nano-grade material preparation
KR20180121102A (en) * 2017-04-28 2018-11-07 메탈페이스 주식회사 A manufacturing method of a flake type zinc powder slurry treated from anti-oxidization
CN110508825A (en) * 2019-09-16 2019-11-29 湖南昊宏新材料科技有限公司 A kind of method that wet ball grinding prepares ultra-fine flakey zinc-bearing alloy powder and products thereof and purposes

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102248176A (en) * 2011-07-15 2011-11-23 云南铜业科技发展股份有限公司 Preparation method of flake silver powder with low burning loss
CN102392254A (en) * 2011-10-31 2012-03-28 西安理工大学 Water-soluble corrosion inhibitor and method for preparing zinc slurry by using the same
CN103204525A (en) * 2012-01-17 2013-07-17 上海杰事杰新材料(集团)股份有限公司 Application of lactam as solvent in nano-grade material preparation
KR20180121102A (en) * 2017-04-28 2018-11-07 메탈페이스 주식회사 A manufacturing method of a flake type zinc powder slurry treated from anti-oxidization
CN110508825A (en) * 2019-09-16 2019-11-29 湖南昊宏新材料科技有限公司 A kind of method that wet ball grinding prepares ultra-fine flakey zinc-bearing alloy powder and products thereof and purposes

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
曲选辉: "硬质合金生产原理和质量控制", 北京:冶金工业出版社, pages: 130 - 131 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115650196A (en) * 2022-09-09 2023-01-31 株洲冶炼集团股份有限公司 Synthesis method of zinc metaphosphate and application of zinc metaphosphate in thallium removal of zinc sulfate solution

Similar Documents

Publication Publication Date Title
CN108080649B (en) Method for preparing superfine iron powder by low-temperature hydrocarbon duplex reduction
CN101628338B (en) Superfine iron-copper alloy powder and preparation method thereof
CN114042920A (en) Superfine flaky zinc powder and preparation process thereof
KR20170088924A (en) Method for producing a cathode material and special cathode material
CN107792891B (en) Preparation method of nickel cobalt lithium manganate powder
CN103357867B (en) A kind of Scale-like multi-component zinc aluminum silicon alloy powder and preparation method thereof
CN105798316A (en) Processing technology of nanoscale tungsten powder
CN107353711B (en) Preparation method of nano particle reinforced resin lead core
CN111872414B (en) Preparation method of micro-nano pre-alloyed powder
CN102259928B (en) Method for preparing Mn3O4 nano-particles
CN115057622B (en) Flake glass, anticorrosive material, anticorrosive coating and preparation method thereof
CN115821064A (en) Low-temperature reduction method for antimony oxide
CN114105184B (en) Method for preparing small-size zinc oxide from carbon dioxide
CN1789461A (en) Method for preparing tungsten carbide-cobalt nano composite powder by low-temperature carbonization of solid carbon
CN104651601A (en) Process for producing reduced ilmenite for welding rod through microwave heating
CN108624771A (en) A method of preparing nano-oxide particles enhancing metallic composite
CN109019668B (en) Method for preparing superfine active zinc oxide powder by hot ball milling oxidation
CN114535591A (en) Method for preparing alloy powder based on surface nanocrystallization treatment
CN112424116B (en) Method for producing lithium cobalt phosphate and method for producing lithium cobalt phosphate carbon composite
CN107130147A (en) The aluminium alloy conductor material and preparation method of a kind of high conductivity
CN114436314A (en) Preparation method of nano yttrium oxide, nano yttrium oxide and yttrium oxide micron hollow sphere
CN113118450A (en) Preparation method of nano-scale and submicron-scale metal powder
WO1994019283A1 (en) Soft ferrite raw material powder and sintered body thereof, and method for producing the same
CN111313024A (en) Nano-lithium magnesium silicate coated high-nickel cathode material and preparation method and application thereof
CN103433480B (en) Scale-like multi-component zinc aluminum silicon alloy powder containing La, Pr and Nd and preparation method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination