CN102701174A - Superfine processing and grain diameter control method of powder materials - Google Patents
Superfine processing and grain diameter control method of powder materials Download PDFInfo
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Abstract
The invention discloses a superfine processing and grain diameter control method of powder materials, wherein inorganic superfine powder material with different grain diameters can be obtained through selecting the type of a processing device, designing the technological process and controlling the technological condition, and thus the method is applicable to the field of large-scale processing preparation of superfine powder. The method disclosed by the invention comprises the following steps of: preparing a dispersion solution with a certain concentration by using inorganic powder, a solvent, a dispersant, an emulsifier and a pH regulator according to proportions, grinding the dispersion solution for a certain time by a physical mechanical grinding process to refine and unify the inorganic powder, adopting a fluid drying and airflow breaking technology to obtain the inorganic superfine powdered materials with different grain diameters. According to the method disclosed by the invention, the granule distribution of the superfine powder is effectively controlled, submicron or nanometer superfine powder can be prepared, the inorganic powder materials such as natural minerals can be processed in a superfine manner, the device size is small, the technological process is convenient, the pollution to the environment is little, and the large-scale processing production of various powder materials is carried out easily.
Description
Technical field
The present invention relates to the preparation and the complete processing of powder body material, particularly a kind of superfine powdery material complete processing and the powder granule controlled method that distributes can be used for the mass-producing processing and preparing field of superfine powder.
Background technology
Ultra-fine powder technology is 20th century new branch of science that grow up of the mid-1970s; Superfine powder is because superfine, the specific surface area of granularity is big and be evenly distributed; Defective is few in addition; Thereby possess many new excellent properties; For example surfactivity is high, speed of reaction is fast, solubleness is big, sintering temperature is low and sintered compact intensity is high, the filler reinforcement performance is good, have unique light, electricity, magnetic property etc. again, and being widely used in not only has irreplaceable effect in high-tech area in high-grade paint, medicine, high-performance ceramics, microelectronics and information material, senior fire-resistant and the economic industry of the people that lagging material, filler and novel material etc. are nearly all; Simultaneously, also brought vigor and vitality to conventional industries.It is the basis of transforming and promote new industry development such as paint, information recode medium, fine ceramics, electronic technology, novel material and biotechnology, is the starting point of modern high technology, occupies critical role in the industry in modern times.
At present superfine powdery material mainly comprises micron, submicron and a small amount of nano-powder, and its preparation approach mainly is divided into three kinds of liquid phase method, vapor phase process and solid phase methods.
Liquid phase method comprises the precipitator method, alkoxide hydrolysis, sol-gel method, electrochemical decomposition method, spray-drying process and freeze-drying etc.Liquid phase method is the working method of at present the most frequently used superfine powder; The equipment and technology flow process is comparatively simple; Cost is lower; But have shortcomings such as the difficult control of the pollutant emission such as a large amount of waste gas and waste liquid and the technological process of production, and this technology can't carry out super-refinement to powder body materials such as natural mineral and process, have certain limitation.
Vapor phase process comprises gas-phase chemical reaction method (CVD), vacuum vapor deposition method (PVD), pasta method of evaporation (VEROS) and plasma method etc.It is little that the product of vapor phase process preparation has a particle diameter, granularity with form evenly, purity advantages of higher, but this method needs equipment huge and complicated, operational requirement is higher, and cost is high, is difficult to promote.
Solid phase method comprises mechanical crushing method, ultrasonic grinding method, thermal decomposition method and explosion method etc.Simple, low cost and other advantages that solid phase method has, but exist product cut size big, surmise and form inhomogeneous, be prone to sneak into shortcoming such as impurity.The mechanical process superfine technique belongs to solid phase method superfine powder manufacturing technology; It is a kind of inorganic superfine powder body material manufacturing method with versatility; Thereby technological core is to realize the super-refinement to material through the means such as impact, collision, shearing and dispersion to material, is one of important means of industrial mineral and other starting material deep processing.But adopt the difficult control of size distribution of the superfine powder of present mechanical crushing process preparation, process of lapping can reduce the purity of material, generally can only produce the superfine powdery material about 5000 orders, can't prepare the superfine powder of submicron or nanoscale.
Summary of the invention
In order to solve the prior art problem; The objective of the invention is to overcome the defective that prior art exists; And provide a kind of super-refinement of powder body material to process and the particle diameter control method; Through to processing units type selecting, process design and processing condition control, obtain the inorganic superfine powder body material of different-grain diameter.The invention solves the deficiency of prior art mechanical process superfine grinding method; Can effectively control the size distribution of superfine powder, can prepare the superfine powder of submicron or nanoscale, can carry out super-refinement processing inorganic powder materials such as natural mineral; Equipment scale is little; Technical process is easy, and environmental pollution is little, is easy to multiple powder body material is carried out the mass-producing processing.
For reaching the foregoing invention purpose, the present invention adopts following technical proposals:
A kind of super-refinement processing and particle diameter control method of powder body material, this method may further comprise the steps:
A. with the suspension-s blend method with powder body material to be processed, solvent and dispersion agent uniform mixing, prepare the dispersion liquid of powder body material to be processed, powder body material wherein to be processed and solvent all should satisfy following prerequisite:
1. low chemically reactive: in air ambient, do not have chemical reaction, the chemical reaction of any character neither takes place between powder body material to be processed and the solvent, the physical reaction of any character does not take place yet; At least can not bonding between powder body material to be processed and the solvent, dissociate, reaction such as swelling, esterification, hydrolysis, complexing, polymerization;
2. low-solubility: powder body material to be processed has insoluble or microsolubility with respect to solvent;
The present invention also preferably adds auxiliary agent in dispersion liquid, auxiliary agent comprises emulsifying agent at least, and uses the high speed homogenization mulser that powder body material to be processed is fully disperseed; Said auxiliary agent also further preferably includes pH value regulator, in dispersion liquid, behind the adding pH value regulator, also uses the high speed homogenization mulser that powder body material to be processed is further fully disperseed;
B. adopt the mechanical process complete processing that dispersion liquid is ground, make further refinement of powder body material to be processed and homogenizing in the dispersion liquid, obtain the powder body material slurries of the further refinement of powder body material to be processed; The preferred wet method mechanical grinding device that adopts carries out the mechanical process attrition process to the powder body material to be processed in the dispersion liquid; The wet method mechanical grinding device is preferably any one or any two or more equipment in vertical grinding machine, horizontal sand mill, planetary ball mill, agitated ball mill and the high energy ball mill; Wet method mechanical mill medium is preferably any one in agate ball, abrasion-proof steel ball, zirconium white microballon, compound zirconia microballon, zirconium silicate microballon, the silit microballon; The grinding chamber cylinder inboard wall material of wet method mechanical grinding device is preferably urethane or zirconia ceramics;
C. with obtaining filtrating behind the powder body material dope filtration, the volatiles evaporation during employing fluid drying method will be filtrated stays the dried powder particle; Preferably adopt the screen filtration powder body material slurries of 800～1000 meshes; Volatiles evaporation during employing fluid drying equipment will be filtrated, the fluid drying evaluation method selecting optimal equipment is centrifugal atomizing drying machine or air-flow jet dryer;
D. adopt airflow pulverization method that the dried powder particle is proceeded to pulverize, obtain the super-refinement powder body material particle of different-grain diameter, and super-refinement powder body material particle is carried out classification according to the size rank take in; The preferred fluidized-bed that adopts is pulverized the dried powder particle spray formula micronizer mill.
The super-refinement processing of powder body material of the present invention and the powder body material to be processed of particle diameter control method processing are any one powder body material in MOX, non-metallic minerals, insoluble salt, high molecular polymer and the metal-powder.
The super-refinement processing of powder body material of the present invention and the solvent that the particle diameter control method is used are water, low volatility alcohols or low volatility alcohol solution.
The present invention has following conspicuous outstanding substantive distinguishing features and remarkable advantage compared with prior art:
1. processing of the super-refinement of powder body material of the present invention and particle diameter control method are mixed with certain density dispersion liquid with auxiliary agents such as inorganic powder, solvent, dispersion agent and emulsifying agent, pH value regulators by proportioning; Adopt physics method mechanical milling tech that dispersion liquid is ground certain hour; Make inorganic powder refinement and homogenizing; Adopt fluid drying and air-flow crushing technology to obtain the inorganic powder material of different-grain diameter, have that production efficiency height, material receive that outside contamination is little, particle size range is controlled, even particle size distribution, environmental pollution are few, be easy to characteristics such as mass-producing processing;
2. compare liquid phase method, the super-refinement processing and the pollutant emission of particle diameter control method of powder body material of the present invention are few, and the technological process of production is easy to control, can carry out super-refinement processing to powder body materials such as natural mineral, are widely used;
3. compare vapor phase process, the super-refinement processing of powder body material of the present invention and preparation technology's equipment of particle diameter control method are comparatively simple, easy to operate, and cost is lower, is easy to promote;
4. compare main solid phase method; Especially the inorganic superfine powder body material manufacturing method of versatility; The size distribution that the super-refinement processing of powder body material of the present invention and particle diameter control method can effectively be controlled superfine powder; The purity of material can be guaranteed, the superfine powder of submicron or nanoscale can be prepared.
Description of drawings
Fig. 1 is the size distribution figure after the super-refinement of a pair of poly-phosphate of embodiment of the invention powder body material to be processed is processed.
Fig. 2 is the size distribution figure after the super-refinement of two pairs of white lake powder body materials to be processed of the embodiment of the invention is processed.
Fig. 3 is the size distribution figure after the super-refinement of three pairs of titanium oxide powder body materials to be processed of the embodiment of the invention is processed.
Embodiment
In conjunction with accompanying drawing, details are as follows to the preferred embodiments of the present invention:
Embodiment one:
The super-refinement processing and the particle diameter CONTROL PROCESS of poly-phosphate:
1) ethanol and water are mixed with 50% spirituous solution by the mass ratio of 1:1, add the dispersion agent of spirituous solution quality 0.2% then, disperse 5min with the high speed homogenization mulser;
2) add the poly-phosphate (2500 order) of spirituous solution quality 25%, and the pH that uses 10% phosphoric acid solution to regulate dispersion liquid is 3 ~ 4, with high speed homogenization mulser dispersion 15min;
3) use horizontal recirculation system sand grinding machine to be the wet method mechanical grinding device, grinding chamber cylinder inboard wall material is a urethane, is grinding medium with the compound zirconia microballon of 0.6 ~ 0.8mm, the liquid flow rate of 0.5L/min, the grinding rate of 2500rpm, circular grinding 2 hours;
4) slurries after will grinding with 800 screen filtrations after, dry with the centrifugal atomizing drying machine;
5) the gained powder particle is pulverized spray formula micronizer mill through fluidized-bed.
The median size of the ultra-fine poly-phosphate that present embodiment is prepared is 200 ~ 300nm, sees the size distribution figure after the super-refinement processing of Fig. 1 poly-phosphate.
Embodiment two:
The super-refinement processing and the particle diameter CONTROL PROCESS of white lake:
1) water and the mass ratio of white lake (1250 order) by 30% are mixed with aqueous dispersions, add the dispersion agent of dispersion liquid quality 0.5% then, disperse 5min with the high speed homogenization mulser;
2) use horizontal recirculation system sand grinding machine to be the wet method mechanical grinding device, grinding chamber cylinder inboard wall material is a urethane, is grinding medium with the compound zirconia microballon of 0.8 ~ 1.0mm, the liquid flow rate of 0.5L/min, the grinding rate of 2500rpm, circular grinding 3 hours;
3) slurries after will grinding with 800 screen filtrations after, dry with the centrifugal atomizing drying machine;
4) the gained powder particle is pulverized spray formula micronizer mill through fluidized-bed.
The median size of the ultrafine aluminium hydroxide that present embodiment is prepared is 400 ~ 600nm, sees the size distribution figure after the super-refinement processing of Fig. 2 white lake.
Embodiment three:
The super-refinement processing and the particle diameter CONTROL PROCESS of white titanium pigment:
1) water and terepthaloyl moietie are mixed with 20% the aqueous solution by the mass ratio of 4:1, add the dispersion agent of solution quality 0.5% then, disperse 5min with the high speed homogenization mulser;
2) pH that uses 10% sodium hydroxide solution to regulate dispersion liquid is 9 ~ 10, add then solution quality 30% white titanium pigment (400 ~ 500nm), with high speed homogenization mulser dispersion 15min;
3) use vertical grinding machine to be the wet method mechanical grinding device, grinding chamber cylinder inboard wall material is a zirconia ceramics, is grinding medium with the compound zirconia microballon of 0.1 ~ 0.2mm, and the grinding rate of 4000rpm ground 5 hours;
4) after the slurries after will grinding filter with 1000 eye mesh screens, with centrifugal atomizing drying machine drying;
5) the gained powder particle is pulverized spray formula micronizer mill through fluidized-bed.
The median size of the superfine titanium white that present embodiment is prepared is 100 ~ 150nm, sees the size distribution figure after the super-refinement processing of Fig. 3 titanium oxide.
Combine accompanying drawing that the embodiment of the invention is illustrated above; But the invention is not restricted to the foregoing description; Can also make multiple variation according to the purpose of innovation and creation of the present invention; Change, the modification of making under all spirit and principles according to technical scheme of the present invention, substitute, combination, simplify, all should be the substitute mode of equivalence, as long as goal of the invention according to the invention; Only otherwise deviate from the super-refinement processing of powder body material of the present invention and the know-why and the inventive concept of particle diameter control method, all belong to protection scope of the present invention.
Claims (12)
1. the super-refinement of a powder body material is processed and the particle diameter control method, it is characterized in that this method may further comprise the steps:
A. with the suspension-s blend method with powder body material to be processed, solvent and dispersion agent uniform mixing, prepare the dispersion liquid of powder body material to be processed, powder body material wherein to be processed and solvent all should satisfy following prerequisite:
1. low chemically reactive: in air ambient, do not have chemical reaction, the chemical reaction of any character neither takes place between powder body material to be processed and the solvent, the physical reaction of any character does not take place yet;
2. low-solubility: powder body material to be processed has insoluble or microsolubility with respect to solvent;
B. adopt the mechanical process complete processing that dispersion liquid is ground, make further refinement of powder body material to be processed and homogenizing in the dispersion liquid, obtain the powder body material slurries of the further refinement of powder body material to be processed;
C. with obtaining filtrating behind the powder body material dope filtration, the volatiles evaporation during employing fluid drying method will be filtrated stays the dried powder particle;
D. adopt airflow pulverization method that the dried powder particle is proceeded to pulverize, obtain the super-refinement powder body material particle of different-grain diameter, and super-refinement powder body material particle is carried out classification according to the size rank take in.
2. the super-refinement of powder body material according to claim 1 is processed and the particle diameter control method, and it is characterized in that: said powder body material to be processed is any one powder body material in MOX, non-metallic minerals, insoluble salt, high molecular polymer and the metal-powder.
3. the super-refinement of powder body material according to claim 1 is processed and the particle diameter control method, and it is characterized in that: said solvent is water, low volatility alcohols or low volatility alcohol solution.
4. process and the particle diameter control method according to the super-refinement of any described powder body material in the claim 1～3; It is characterized in that: in step a; Also in dispersion liquid, add auxiliary agent, auxiliary agent comprises emulsifying agent at least, and uses the high speed homogenization mulser that powder body material to be processed is fully disperseed.
5. the super-refinement of powder body material according to claim 4 is processed and the particle diameter control method; It is characterized in that: said auxiliary agent also comprises pH value regulator; After in dispersion liquid, adding pH value regulator, also use the high speed homogenization mulser that powder body material to be processed is further fully disperseed.
6. according to the super-refinement processing and the particle diameter control method of any described powder body material in the claim 1～3, it is characterized in that: in step c, adopt the screen filtration powder body material slurries of 800～1000 meshes.
7. process and the particle diameter control method according to the super-refinement of any described powder body material in the claim 1～3; It is characterized in that: in step c; Volatiles evaporation during employing fluid drying equipment will be filtrated, fluid drying equipment is centrifugal atomizing drying machine or air-flow jet dryer.
8. according to the super-refinement processing and the particle diameter control method of any described powder body material in the claim 1～3, it is characterized in that: in steps d, adopt fluidized-bed that spray formula micronizer mill is pulverized the dried powder particle.
9. according to the super-refinement processing and the particle diameter control method of any described powder body material in the claim 1～3, it is characterized in that: in step b, adopt the wet method mechanical grinding device that the powder body material to be processed in the dispersion liquid is carried out the mechanical process attrition process.
10. the super-refinement of powder body material according to claim 9 processing and particle diameter control method is characterized in that: said wet method mechanical grinding device is any one or any two or more equipment in vertical grinding machine, horizontal sand mill, planetary ball mill, agitated ball mill and the high energy ball mill.
11. processing of the super-refinement of powder body material according to claim 10 and particle diameter control method, it is characterized in that: said wet method mechanical mill medium is any one in agate ball, abrasion-proof steel ball, zirconium white microballon, compound zirconia microballon, zirconium silicate microballon, the silit microballon.
12. processing of the super-refinement of powder body material according to claim 10 and particle diameter control method, it is characterized in that: the grinding chamber cylinder inboard wall material of said wet method mechanical grinding device is urethane or zirconia ceramics.
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| CN106543627A (en) * | 2016-10-18 | 2017-03-29 | 成都新柯力化工科技有限公司 | A kind of high-temperature resistance plastice lubricating additive and preparation method thereof |
| CN106946576A (en) * | 2017-04-12 | 2017-07-14 | 潮州三环（集团）股份有限公司 | A kind of method that ceramic powder is prepared with ceramic solid waste |
| CN108554538A (en) * | 2018-05-19 | 2018-09-21 | 西安博尔新材料有限责任公司 | A kind of preparation method of silicon carbide medium ball |
| CN109167044A (en) * | 2018-09-12 | 2019-01-08 | 山西中电科新能源技术有限公司 | The method for preparing lithium cell cathode material using Buddha's warrior attendant wire cutting waste silicon powder |
| CN110526295A (en) * | 2019-07-16 | 2019-12-03 | 东北大学 | One kind mixing ytterbium Gadolinium Tungstate potassium nano crystal particles and preparation method thereof |
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| CN109167044A (en) * | 2018-09-12 | 2019-01-08 | 山西中电科新能源技术有限公司 | The method for preparing lithium cell cathode material using Buddha's warrior attendant wire cutting waste silicon powder |
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| CN110526295B (en) * | 2019-07-16 | 2021-05-14 | 东北大学 | Ytterbium-doped potassium gadolinium tungstate nanocrystal particle and preparation method thereof |
| CN113118450A (en) * | 2019-12-31 | 2021-07-16 | 拓米(成都)应用技术研究院有限公司 | Preparation method of nano-scale and submicron-scale metal powder |
| CN114394831A (en) * | 2022-01-07 | 2022-04-26 | 河北欧禹科技有限公司 | Solid electrolyte and method for producing same |
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Application publication date: 20121003 |