CN100446863C - Manufacturing method of nanometer squama and special equipment thereof - Google Patents
Manufacturing method of nanometer squama and special equipment thereof Download PDFInfo
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- CN100446863C CN100446863C CNB2005101191401A CN200510119140A CN100446863C CN 100446863 C CN100446863 C CN 100446863C CN B2005101191401 A CNB2005101191401 A CN B2005101191401A CN 200510119140 A CN200510119140 A CN 200510119140A CN 100446863 C CN100446863 C CN 100446863C
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Abstract
The invention belong to the field of superfine powder processing and nano-powder processing, specially it is the preparation methods and equipment for nano-scale materials or nano-scale composite materials, the invention solved the problems of high costs, low efficiency, low quality in powders fine processing. The invention make the usual process of ultrafine steps - crushed, mixed, decentralization, surface treatment, modification, releasing step and nanopowder synthesis simplified merger, make one step produce the nano-scale materials come ture by using proprietary equipment 'planetary ball mill which the revolution and rotation speed can be adjust'. The thickness of Nano-scale is 10 ~ 100 nm, radial size ranged from 0.5 to 50 mu m, is one-dimensional nanomaterials, overcoming the secondary combination step problems in conventional ultrafine powder processing, and easy to spread in different use occasions.
Description
Technical field
The invention belongs to powder super-fine processing and nano-powder manufacture field, the preparation method and the special equipment thereof of a kind of specifically nanometer scale material or nanometer scale composite.
Background technology
Along with progress of science and technology, the powder industry development enters into the nanoscale field, and this is one of trend of international powder technology development.In the development that becomes more meticulous, the important function of industrial powder deep process technology in scientific research and industrial production embodies more and more fully at world's powder industry.Starting with from disintegrating apparatus in countries in the world, expands to many aspects such as super-fine classified, high evenness mixing, surface treatment, nano powder preparation gradually.
In recent years, the powder industry of China is also followed the development of powder technology and is popularized and the formation scale.Because the every aspect that relates to industrial circle is handled in the processing of solid material, comprehensive industrial technology characteristic, for powder industry has brought vigor, inter-trade technological diffusion makes that also powder technology market is vigorous.
Yet China is also quite backward aspect powder technology.In recent years, in industries such as magnetic pipe recording material, electronic ceramics, high-grade paint, printing ink, coating, plastics, rubber, having introduced more than ten covers is the machining production line of raw material with the ultrafine inorganic powder material, wherein many have an international most advanced level, but do not set up supporting with it superfine powdery material industry so far as yet, superfine powdery material is still mainly by import.For example, ultramicro grinding split pole technology and equipment is quite ripe abroad, and domestic also being in from research to industrialized transition stage; The kind of powder product of becoming more meticulous is few, output is little, of low quality, can not satisfy the requirement of new high-tech industry to raw material; The powder complex technique of high request also is in the research and development stage; The application of auxiliary agent and pulverizing are lower with the integration of operation level of other chemical engineering unit operation; Much must still rely on introduction overseas equipment and technology to solve problem with the field of the powder product that becomes more meticulous, some then need buy external product; Chemical method, prepared by physical method superfine powder and nano-powder technology engender, but because of costs such as energy consumption height is difficult to large-scale industrial production, its application technology is still waiting exploitation; The industry of domestic application ultrafine powder, owing to lack the high-quality powder material make its product still rest on low-level on; To state's outer vent as some nonmetal mineral product, also cheap selling causes the loss of resource owing to lack working ability.The nanometer scale technology of preparing is a kind of efficient superfine powder and nano-powder process technology, and the powder active height of processing, cost is low, efficient is high, can satisfy the requirement of every profession and trade to superfine powder.
The prospect of China's development superfine powder and nano-powder industry is very good.At first there are abundant powder industry raw material and market in China.Along with the adjustment of country's industrial structure, all kinds of new products constantly occur under the support of new technology, and becoming more meticulous of raw material makes domestic increase in demand to superfine powder and nano-powder product.Only at coating industry, coating reached 180,000 tons in 2000 with titanium dioxide, 450,000 tons of coating kaolins, and industries such as plastic filler, gum filler, rubber filling, coating, printing ink, dyestuff, medicine, daily use chemicals are very fast to the increase in demand of high activity fine powder product.
The invention enables high evenness mixing, surface treatment, one step of nanometer scale preparation to finish, for a new road has been opened up in the powder deep processing.Its thickness of nanometer scale of the present invention is 10～100nm, and radial dimension is 0.5～50 μ m, is monodimension nanometer material.Be mainly used in the active filler of coating, rubber, plastic or other material, be used to improve, improve mechanical performance, chemical property, the physical property of material, produce high performance material.
Summary of the invention
The technical issues that need to address of the present invention:
The objective of the invention is in order to solve difficult problems such as cost height, efficient in the powder retrofit is low, quality is low, common superfining process step is pulverized one by one, mixed, dispersion, surface treatment, modification, separates rapid and synthetic simplification of nano-powder merges, realize that one-step method makes the nanometer scale material.The thickness of nanometer scale is 10～100nm, and radial dimension is 0.5～50 μ m, is monodimension nanometer material.Overcome in the conventional superfine powder process superfine powder secondary simultaneously and roll into a ball a rapid difficult problem, and be easy to disperse in different use occasions.
The technical solution used in the present invention is:
The present invention is that the task equipment " planetary ball mill of revolution, the equal adjustable speed of rotation " that adopts inventor's design is implemented, this task equipment replaces the gravitational field of general milling with the field of force that is multiple times than acceleration of gravity, existing revolution has rotation again during mill tube (planet work cylindrical shell) work, abrading-ball is under the effect that rotation, revolution etc. is made a concerted effort, centrifugal acceleration can reach 10～20 times of acceleration of gravity even higher, and abrading-ball rotates at a high speed under the frictional force effect, during collision material is produced very strong shearing, abrasive action.Material is realized pulverizing, is mixed under means effects such as the mutual impact of abrading-ball and abrading-ball, abrading-ball and mill tube, friction, shearing, bending, extension, extruding, grinding, dispersion, surface treatment, modification, subtract rapid and nano-powder synthetic.
Being constructed as follows of the planetary ball mill machine equipment of revolution, the equal adjustable speed of rotation:
. this ball mill equipment comprises the vibration damping leg, base, revolution speed change input mechanism, main shaft, bearing, rotary table, bearing, planet work cylindrical shell, pinion, gear wheel, bearing, rotation speed change input mechanism, cooling blower, described main shaft, rotary table, bearing, planet work cylindrical shell, bearing, pinion and gear wheel constitute the rotating part of complete machine, the rotating part of complete machine is by bearing and being set on the base, revolution speed change input mechanism is connected an end of main shaft, main shaft is provided with two rotary tables, uniform on the concentric circumferences of rotary table a plurality of planet work cylindrical shells are set, one end of each planet work cylindrical shell has pinion, rotation speed change input mechanism is by gear wheel and pinion, the vibration damping leg is installed below base, the corresponding planet seating nipple of the air channel air opening end body setting that is provided with in the base, the other end links to each other with cooling blower.
The method that employing the said equipment prepares nanometer scale is as follows:
1, at first take by weighing processing materials by 6～15% of work cylindrical shell volume, the particle diameter of material is at 100～400 orders, and material can be metal powder or metal oxide powder or mineral powder or organic matter powder or other non-metal powder etc.
2, choose abrading-ball by work cylindrical shell volume and material variety, material is 1: 2～5 with the ratio of abrading-ball volume, grinding ball material and material material will be complementary, can be bearing steel or stainless steel or agate or pottery or titanium or steel alloy or diamond or cast stone etc., sphere diameter 3～30mm, the big or small proportioning of ball is decided according to different material, in order to increase the collision frequency of abrading-ball, generally choosing the abrading-ball that is no less than three kinds of dimensions, is (13/16) such as the specification of bearing steel ball "; (19/32) "; (3/8) "; (5/16) "; (7/32) " five kind.
3, take by weighing dispersant, protective agent and solvent by weight of material, general dispersant accounts for 0.1～3% of weight of material; Protective agent accounts for 0.5～10% of weight of material; Solvent accounts for 150～600% of weight of material.Described dispersant is one or more of triethanolamine or surfactant etc.; Protective agent is one or more of the compound that contains more unsaturated double-bond such as polysulfide rubber, resin and plastics; Solvent is one or more of ethanol, butanols, acetone, dimethylbenzene, toluene, ethyl acetate and water etc.
4, material, abrading-ball, dispersant, protective agent and solvent in above-mentioned 1,2,3 are rendered in the work cylindrical shell, wherein the cumulative volume of material, abrading-ball, dispersant, protective agent and solvent accounts for 50～90% of work cylindrical shell volume.
5, to add the revolution speed of adjusting " planetary ball mill of revolution, the equal adjustable speed of rotation " man-hour be 300～600r/min to nanometer scale, and rotational velocity is 800～2400r/min.
6, nanometer scale process time is 2～6 hours.
Operate by above. to its thickness is 10～100nm, radial dimension is the 1-dimention nano scale material of 0.5～50 μ m.
The present invention has the following advantages and good effect
1, nanometer scale preparation methods of the present invention has solved cost height in the powder retrofit, low, the low-quality problem of efficient, this method is with common superfining process step---pulverizing, mixing, dispersion, surface treatment, modification, separate rapid and synthetic etc. the simplification of nano-powder merges, realize that one-step method makes the nanometer scale material---its thickness is 10～100nm, radial dimension is 0.5～50 μ m, is monodimension nanometer material.
2, this method overcomes in the conventional superfine powder process superfine powder secondary simultaneously and rolls into a ball a rapid difficult problem, does not roll into a ball suddenly, and is easy to disperse in different use occasions.
3, product of the present invention can be widely used in plastics, rubber, rubber and plastic, coating, printing ink, dyestuff, for example, after adding nanometer scale in the coating, its nanometer scale and resin form chemisorbed or chemical bonding, can make coating form solid netted overall structure and have good adhesive force, good permeability resistance, high anti-corrosive properties and some specific functions.
4, plastic filler, gum filler, rubber filling, coating, printing ink, dyestuff are dosed this nanometer scale material the performance of matrix material are greatly improved.
Description of drawings
Fig. 1 is the special equipment revolution of preparation nanometer scale, the planetary ball mill overall structure schematic diagram of the equal adjustable speed of rotation.
Fig. 2,3,4 is varying number work cylindrical shell distribution situation structural representation on the rotary table of the present invention.
The specific embodiment
By shown in Figure 1: this ball mill equipment comprises vibration damping leg (1), base (2), revolution speed change input mechanism (3), main shaft (4), bearing (5), rotary table (6), bearing (7,9), planet work cylindrical shell (8), pinion (10), gear wheel (11), bearing (12), rotation speed change input mechanism (13), cooling blower (14), described main shaft (4), rotary table (6), bearing (7), planet work cylindrical shell (8), bearing (9), pinion (10) and gear wheel (11) constitute the rotating part of complete machine, the rotating part of complete machine is set on the base (2) by bearing (5) and (12), revolution speed change input mechanism (3) is connected an end of main shaft (4), main shaft (4) is provided with two rotary tables (6), the uniform a plurality of planet work cylindrical shells (8) that are provided with on the concentric circumferences of rotary table (6), one end of each planet work cylindrical shell (8) has pinion (10), rotation speed change input mechanism (13) is by gear wheel (11) and pinion (10) engagement, vibration damping leg (1) is installed below base (2), the corresponding planet seating nipple body of air channel (15) air opening end (8) that is provided with in the base (2) is provided with, and the other end links to each other with cooling blower (14).
Described revolution speed change input mechanism (3), rotation speed change input mechanism (13) constitutes by frequency control motor and frequency conversion electrical control device.
Described planet work cylindrical shell (8) adopts metal, pottery, agate, engineering plastics manufacturing.
Preparation embodiment one:
The planetary ball mill work cylindrical shell volume of this routine employed revolution, the equal adjustable speed of rotation is 460ml, and institute's processing materials is 100 order silica flours, and abrading-ball is a steel ball, and dispersant, protective agent, solvent are respectively triethanolamine, calgon, ethanol.
1, the weight of calculating processing materials silica flour by the volume of work cylindrical shell is 115g.Take by weighing in the 115g silica flour adding work cylindrical shell.
2, the volume by the work cylindrical shell calculates the bearing steel ball (13/16) of selecting five kinds of specifications for use "; (19/32) "; (3/8) "; (5/16) "; (7/32) ".
The weight of various bearing steel balls is respectively (13/16) " 358.2g; (19/32) " 154.7g; (3/8) " 109.5g; (5/16) " 10.1g; (7/32) " 10.6g.
3, the weight that calculates dispersant, protective agent and solvent by weight of material is respectively triethanolamine 10g; Calgon 1g; Ethanol 180g.
Take by weighing triethanolamine 10g; Calgon 1g; Ethanol 180g adds in the work cylindrical shell.
4, will work cylindrical shell sealing is installed on the planetary ball mill of revolution, the equal adjustable speed of rotation, and the adjustment revolution speed is 450r/min; Rotational velocity is 1600r/min.Processing and obtaining thickness in 4 hours is 10～100nm, radially is the silica flour 1-dimention nano scale material of 0.5～50 μ m.
Preparation embodiment two:
The planetary ball mill work cylindrical shell volume of this routine employed revolution, the equal adjustable speed of rotation is 460ml, and institute's processing materials is 200 order iron powders, and abrading-ball is a steel ball, and dispersant, protective agent, solvent are respectively triethanolamine; Calgon; Water.
1, the weight of calculating the processing materials iron powder by the volume of work cylindrical shell is 200g.Take by weighing in the 200g iron powder adding work cylindrical shell.
2, the volume by the work cylindrical shell calculates the bearing steel ball (13/16) of selecting five kinds of specifications for use "; (19/32) "; (3/8) "; (5/16) "; (7/32) ".
The weight of various bearing steel balls is respectively (13/16) " 358.2g; (19/32) " 154.7g; (3/8) " 109.5g; (5/16) " 10.1g; (7/32) " 10.6g.
3, the weight that calculates dispersant, protective agent and solvent by weight of material is respectively triethanolamine 10g; Calgon 1g; Water 200g.
Take by weighing triethanolamine 10g; Calgon 1g; Water 200g adds in the work cylindrical shell.
4, will work cylindrical shell sealing is installed on the planetary ball mill of revolution, the equal adjustable speed of rotation, and the adjustment revolution speed is 450r/min; Rotational velocity is 1600r/min.Processing and obtaining thickness in 4 hours is 10～100nm, and radial dimension is the iron powder 1-dimention nano scale material of 0.5～50 μ m, and this powder can be used for the magnetic flow liquid material.
Preparation embodiment three:
The planetary ball mill work cylindrical shell volume of this routine employed revolution, the equal adjustable speed of rotation is 1820ml, and institute's processing materials is 320 order iron powders, and abrading-ball is a steel ball, and dispersant, protective agent are respectively epoxy resin; Polysulfide rubber, solvent are that dimethylbenzene, acetone, butanols weight ratio are dimethylbenzene: acetone: butanols=2: 1: 2.
1, the weight of calculating the processing materials titanium valve by the volume of work cylindrical shell is 600g.Take by weighing in the 600g titanium valve adding work cylindrical shell.
2, the volume by the work cylindrical shell calculates the bearing steel ball (13/16) of selecting five kinds of specifications for use "; (19/32) "; (3/8) "; (5/16) "; (7/32) ".
The volume of various bearing steel balls is respectively (13/16) " 188.7ml; (19/32) " 86.2ml; (3/8) " 55.6ml; (5/16) " 5.8ml; (7/32) " 5.4ml.
3, the weight that calculates dispersant, protective agent and solvent by weight of material is respectively epoxy resin 42g; Polysulfide rubber 42g; The solvent volume that mixes is 650ml.
Take by weighing epoxy resin 42g; Polysulfide rubber 42g; Measure the solvent 650ml that mixes.In the adding work cylindrical shell.
4, will work cylindrical shell sealing is installed on the planetary ball mill of revolution, the equal adjustable speed of rotation adjustment revolution speed 411r/min; Rotational velocity 1500r/min.Processing and obtaining thickness in 4 hours is 10～100nm, and radial dimension is the titanium valve 1-dimention nano scale material of 0.5～50 μ m.
Claims (4)
1, a kind of preparation method of nanometer scale, it is characterized in that: this method is to adopt a kind of special equipment for preparing nanometer scale, this special equipment comprises vibration damping leg (1), base (2), revolution speed change input mechanism (3), main shaft (4), clutch shaft bearing (5), rotary table (6), second bearing (7), the 3rd bearing (9), planet work cylindrical shell (8), pinion (10), gear wheel (11), the 4th bearing (12), rotation speed change input mechanism (13), cooling blower (14), described main shaft (4), rotary table (6), second bearing (7), planet work cylindrical shell (8), the 3rd bearing (9), pinion (10) and gear wheel (11) constitute the rotating part of described special equipment, the rotating part of described special equipment is set on the base (2) by clutch shaft bearing (5) and the 4th bearing (12), revolution speed change input mechanism (3) is connected an end of main shaft (4), main shaft (4) is provided with two rotary tables (6), the uniform a plurality of planet work cylindrical shells (8) that are provided with on the concentric circumferences of rotary table (6), one end of each planet work cylindrical shell (8) has pinion (10), rotation speed change input mechanism (13) is by gear wheel (11) and pinion (10) engagement, vibration damping leg (1) is installed below base (2), the corresponding planet seating nipple body of air channel (15) air opening end (8) that is provided with in the base (2) is provided with, and the other end links to each other with cooling blower (14);
The concrete steps of this method are as follows:
A, at first take by weighing processing materials by 6～15% of work cylindrical shell volume, the particle diameter of material is at 100～400 orders;
B, choose abrading-ball by work cylindrical shell volume and material variety, material is 1 with the ratio of abrading-ball volume: (2～5), and grinding ball material and material material will be complementary, in order to increase the collision frequency of abrading-ball, choose the abrading-ball that is no less than three kinds of dimensions;
C, take by weighing dispersant, protective agent and solvent by weight of material, dispersant accounts for 0.1～3% of weight of material; Protective agent accounts for 0.5～10% of weight of material; Solvent accounts for 150～600% of weight of material;
D, the material with among above-mentioned a, b, the c, abrading-ball, dispersant, protective agent and solvent are rendered in the work cylindrical shell, and wherein the cumulative volume of material, abrading-ball, dispersant, protective agent and solvent accounts for 50～90% of work cylindrical shell volume;
The revolution speed that e, nanometer scale add the special equipment of adjusting above-mentioned preparation nanometer scale man-hour is 300～600r/min, and rotational velocity is 800～2400r/min;
F, nanometer scale process time is 2～6 hours;
Obtaining its thickness by above operation is 10～100nm, and radial dimension is the 1-dimention nano scale material of 0.5～50 μ m.
2, the preparation method of nanometer scale according to claim 1 is characterized in that: described material is metal powder or metal oxide powder or mineral powder or organic matter powder or other non-metal powder.
3, the preparation method of nanometer scale according to claim 1, it is characterized in that: described grinding ball material is bearing steel or stainless steel or agate or pottery or titanium or steel alloy or diamond or cast stone, sphere diameter 3～30mm, the big or small proportioning of ball is decided according to different material.
4, the preparation method of nanometer scale according to claim 1 is characterized in that: described dispersant is a surfactant; Protective agent is the polysulfide rubber compound that contains unsaturated double-bond, contain the resin compound of unsaturated double-bond and contain one or more of plastic compound of unsaturated double-bond; Solvent is one or more of ethanol, butanols, acetone, dimethylbenzene, toluene, ethyl acetate and water.
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| CNB2005101191401A CN100446863C (en) | 2005-12-31 | 2005-12-31 | Manufacturing method of nanometer squama and special equipment thereof |
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| CNB2005101191401A CN100446863C (en) | 2005-12-31 | 2005-12-31 | Manufacturing method of nanometer squama and special equipment thereof |
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| CN100446863C true CN100446863C (en) | 2008-12-31 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102773134A (en) * | 2011-05-09 | 2012-11-14 | 长春超威医药技术开发有限公司 | High energy horizontal planetary ball milling equipment for production of nanometer traditional Chinese medicine powder |
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Owner name: BAI RIZHONG Free format text: FORMER OWNER: SHENZHEN ZHONGKE SURFACE ENGINEERING TECHNOLOGY CO., LTD. Effective date: 20130606 |
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Free format text: CORRECT: ADDRESS; FROM: 110000 SHENYANG, LIAONING PROVINCE TO: 136001 SIPING, JILIN PROVINCE |
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Effective date of registration: 20130606 Address after: 136001 Siping East District, Siping City, Hebei Province, two north latitude road No. 198 Siping East Sea Petrochemical Equipment Co., Ltd., Jilin Patentee after: Bai Rizhong Address before: 110000 Liaoning city in Shenyang Province town of Long Beach economic and Technological Development Zone West Long Village Patentee before: Shenyang Zhongke Surface Engineering Technology Co., Ltd. |
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Application publication date: 20070704 Assignee: Shenyang Zhongke surface engineering science and Technology Development Co Ltd Assignor: Bai Rizhong Contract record no.: 2013210000073 Denomination of invention: Manufacturing method of nanometer squama and special equipment thereof Granted publication date: 20081231 License type: Exclusive License Record date: 20130712 |
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Assignee: Shenyang Zhongke surface engineering science and Technology Development Co Ltd Assignor: Bai Rizhong Contract record no.: 2013210000073 Date of cancellation: 20151013 |
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