CN1265887C - Method for preparing nanometer ultra-fine tourmaline powder - Google Patents
Method for preparing nanometer ultra-fine tourmaline powder Download PDFInfo
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- CN1265887C CN1265887C CN 200410000816 CN200410000816A CN1265887C CN 1265887 C CN1265887 C CN 1265887C CN 200410000816 CN200410000816 CN 200410000816 CN 200410000816 A CN200410000816 A CN 200410000816A CN 1265887 C CN1265887 C CN 1265887C
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Abstract
The present invention belongs to the field of manufacturing non-metallic mineral powders, particularly to a preparation method for nano grade ultra-fine tourmaline micro powder. The preparation method of the present invention comprises the procedures of raw ore coarse crushing, airflow crushing, powder post-treatment, wet ball milling, spray drying, powder disaggregation, packaging and storage. The preparation method comprises the main technical parameters that primarily crushed tourmaline powder is put in natural air and is calcined at 300 to 800 DEG C, calcination time is 2 to 4 hours so as to obtain the tourmaline powder with different colors, and ball milling time is 36 to 72 hours. Compared with the prior art, the present invention has the advantage of simple technical operation, can obviously decrease the agglomeration of the tourmaline ultra-fine powder and can increase powder crushing efficiency; grain diameters of the powder are obviously reduced to 15 to 60 nm, the generating capacity of negative ions is obviously improved, and the manufactured powder has the advantages of multiple color, no subsequent processing influence, safe use and wide application range.
Description
Technical field
The invention belongs to the preparation field of ultra-fine nonmetallic ore powder, particularly nano level superfine tourmaline micropowder preparing process.
Background technology
In actual life, what of air negative oxgyen ion have become standard whether with fresh air, The World Health Organization's regulation, and the normal concentration of fresh air anion is to be lower than 1000 to 1500 in every cc of air.To the mensuration that bacterial content in 7 the sample point air in Dinghu Hill carries out, found that all be zero, abacterial main cause is that airborne negative oxygen ion has very strong sterilizing power.Yet indoor negative aeroion content such as the city that population is relatively concentrated, office, hotel, hospital is seldom (generally at 100/cm
3Below), it is very muddy that air seems.Along with the raising of people's living standard and the development of modern medicine, human hope becomes pure and fresh as the Nature with the air in own room, that is to say the concentration that will improve anion in the room air.
Anion generator has appearred in earlier 1990s on the market, this anion generator mainly is to utilize the electrion effect, when producing anion, supervenes harmful substances such as ozone and oxynitrides, thereby the market of fading out very soon.Afterwards, it is found that natural mineral tourmaline have piezoelectricity, electrically forever, pyroelectricity, can make the characteristic of surrounding air negative ionization and hydrone moment negative ionization, also has emitting far-infrared characteristic, therefore cause people's extensive concern, natural be considered to a kind of natural anion generator.Tourmaline is nontoxic, the safe natural minerals of a kind of ring silicate, and its chemical molecular formula is: XY
3Z
6[Si
6O
18] (O, OH, F)
4(X=Ca, K, Na; Y=Fe
2+, Mg
2+, Al, Li, Fe
3+, Mn
2+Z=Al, Cr
3+, Fe
3+), because tourmaline hardness is big, mohs hardness 7～7.5; The super-fine processing difficulty in process, after being crushed to 10 μ m, powder viscosity strengthens (may be charged relevant with tourmaline crystal two ends), and crush efficiency reduces.Have a strong impact on the performance performance and the subsequent applications of ultrafine powder, especially in the application of aspects such as weaving, cosmetics, and only be worked into super fine (reaching nanoscale), just can give full play to it and discharge anion, far function, and not influence following process.From the relevant patent of present application, the overwhelming majority is that the Application of composite of tourmaline powder (as CN 1307077A, discloses a day 2001.8.8; CN 1089326C, open day 2002.8.21; CN 1242943A, open day 2000.2.2; The open day 1999.7.14 of CN 1222494A etc.), seldom relate to tourmaline powder ultra micro processing technology, post processing etc., and used diameter of particle is also bigger; What have has related to the powder processing technology, as CN 1287888A (open day 2001.3.21), CN 1425503A (open day 2003.6.25) has narrated a kind of tourmaline micropowder preparing process, related to the ultra micro processing technology of powder, but its complex process, the color of being produced single (black), influencing the scope of application and following process handles, as the dyeing etc. of weaving, the particle diameter of its production is also bigger than normal, is unfavorable for the application of powder at aspects such as weaving, cosmetics.And the patent of invention that has has been added rare earth, catalysis material etc. in order to improve the performance of powder, and prepared composite granule exists bigger potential safety hazard.
Summary of the invention
The object of the present invention is to provide a kind of technological operation easy, can obviously reduce the reunion of tourmaline ultrafine powder, improve crush efficiency, make diameter of particle obviously be reduced to particle diameter 15～60nm, the anion generating ability obviously improves, and the powder color diversity of producing does not influence following process, nano level superfine tourmaline micropowder preparing process safe in utilization, that have wide range of applications.
Preparation method's of the present invention technological principle is the tourmaline ultrafine powder that makes, do not destroy its crystal structure characteristic, in the powder mechanical milling process, effect by power such as the collision between powder and mill Jie, powder and the powder etc., shearings, make its pulverizing, but, be difficult to further pulverize simultaneously owing to the increase of specific area, the effect of Van der Waals force cause powder reuniting.So we by the adding of grinding aid, can reduce the reunion of powder, and pulverize the agglomerated effect by air-flow and further reduce, thereby prepare particle diameter at nano level ultrafine powder.By the powder aftertreatment technology, make the element redox generation variation of valence in the tourmaline in addition, have characteristics such as better release anion, far infrared.
According to above-mentioned purpose and technological principle, the technical scheme that we proposed is as follows:
The technological process of this method comprises that raw ore coarse crushing, air-flow pulverizing, powder post processing, wet ball grinding, spray-drying, powder separate reunion, packaging and storing, and existing division is as follows:
(1) raw ore coarse crushing.The former mining jaw crusher of tourmaline is crushed to the beans shape, and preliminary the pulverizing obtains the particle that particle diameter is 50～60 μ m;
(2) air-flow is pulverized.With ultrafine crusher granular tourmaline is carried out an air-flow and pulverize, obtain the tourmaline powder of particle diameter 10～20 μ m;
(3) powder post processing.To discharge anion etc. functional in order to increase tourmaline powder, and tourmaline powder is placed natural air, and 300 ℃～800 ℃ calcinings down, calcination time is 2～4 hours, and calcining heat and asynchronism(-nization) obtain the tourmaline powder of different colours.And tourmaline powder does not lump, and the crystal structure characteristic of tourmaline powder does not change.
(4) wet ball grinding.To carry out ball milling in the burnt tourmaline powder adding agitating ball mill, ball adds mill and is situated between and grinding aid in order to reduce the reunion of powder in ball milling, ball milling after 36～80 hours through the screening, mill is situated between and stays in the ball mill, can obtain the tourmaline slip of particle diameter 15～60nm, wherein:
Tourmaline powder and the ratio of grinding Jie: 1: 4～1: 6.
The ratio of tourmaline powder and dispersant water: 1: 1～1: 1.5.
The ratio of tourmaline powder and grinding aid is: 1: 0.005～1: 0.05.
(5) spray-drying.Resulting tourmaline slip is dispersed into droplet sprays in the hot blast, moisture content≤1 ‰.Grinding aid decomposes in the time of 300-500 ℃.Through granulation, the tourmaline particle that makes is spherical;
(6) powder is separated reunion.The tourmaline powder that spray-drying is intact joins in the crushing chamber from charging aperture, under the effect of high velocity air, material is by the bump between self particle, air-flow is to the impact of the impact shear effect of material and material and other parts, friction, shearing and make material separate reunion, also play simultaneously certain pulverization, the tourmaline powder particle diameter 15～60nm after secondary gas flow is pulverized.
(7) packaging and storing.With the tourmaline ultrafine powder that processes, to pack on request, deposit in dry frescade.
Tourmaline ultrafine powder preparation method's further feature is that grinding aid is any one in polyacrylate, salt or the polyacrylamide.
Mill Jie is any one in zirconia ball or the alumina balls.
The particle diameter that mill is situated between is 2～5mm.
By technique scheme, obtained nano level superfine tourmaline powder constituent (weight %) be: SiO
2: 35～45%; Al
2O
3: 20～34%; Fe
2O
3(FeO): 10～15%; B
2O
3: 9～11%; MgO:5～8%; Na
2O:1.5～3%; TiO
2: 0.5～1.5%; CaO:0.5～1.5%; K
2O:0.001～0.05%.
It is easy that the present invention compared with prior art has technological operation, can obviously reduce the reunion of tourmaline ultrafine powder, improve crush efficiency, make diameter of particle obviously be reduced to particle diameter 15～60nm, its anion generating ability is obviously improved, and the concentration of anion reaches 1500-3000/cm
3, and the powder color of producing has diversity, do not influence following process, advantage safe in utilization.Also can be widely used in industries such as weaving, coating, filler, water purification through the present invention prepared ultrafine powder, mainly have far infrared, produce anion, purify air and indoor pollution, eliminate the unusual smell, effect such as activated water molecule.
The specific embodiment
Adopt preparation method of the present invention, the technological process according to raw ore coarse crushing, air-flow pulverizing, powder post processing, wet ball grinding, spray-drying, powder are separated reunion, packaging and storing has prepared 4 batches of nano level superfine tourmaline powders that sequence number is 1～4#.Institute's technical matters parameter of having adopted and the coarse crushing of tourmaline raw ore, air-flow pulverize and the ultimate size size is listed in table 1.The composition proportion of the tourmaline in technological process, mill Jie, grinding aid, dispersant is listed in table 2.The chemical composition composition and the color of the prepared nano level superfine tourmaline of the present invention are listed in table 3.Negative ion concentration, far infrared transmissivity that the measured nano level superfine tourmaline of the present invention takes place are listed in table 4.Far infrared is by the test of college of science of University Of Tianjin, and tester is 5DX Fourier transformation infrared spectrometer (production of America NI COLET company), and test condition is: 100 ℃ of constant temperature, environment temperature are 20 ℃.Negative ion concentration is by the test of Shanghai test center, and tester is the air ion concentration measuring apparatus, and test condition is: 20 ℃ of temperature, humidity 45%, environmental chamber.Method of testing: total indicator reading method.
Table 1 technical matters parameter of the present invention and the coarse crushing of tourmaline raw ore, air-flow are pulverized and the ultimate size size table
Tourmaline in table 2 technological process of the present invention, mill Jie, grinding aid, dispersant composition proportion table
The chemical composition composition of the prepared nano level superfine tourmaline powder of table 3 the present invention and color table (weight %)
Nano level superfine tourmaline powder generating negative ions concentration, far infrared transmissivity table that table 4 the present invention is measured
Claims (4)
1, nano level superfine tourmaline micropowder preparing process is characterized in that its technological process comprises that raw ore coarse crushing, air-flow pulverizing, powder post processing, wet ball grinding, spray-drying, powder separate reunion, packaging and storing, and existing division is as follows:
(1) raw ore coarse crushing: the former mining jaw crusher of tourmaline is crushed to the beans shape, the preliminary average grain diameter that obtains 50～60 μ m of pulverizing;
(2) air-flow is pulverized: with ultrafine crusher granular tourmaline is carried out an air-flow and pulverize, obtain the tourmaline powder of average grain diameter 10～20 μ m;
(3) powder post processing: tourmaline powder is placed natural air, and 300 ℃～800 ℃ calcinings down, calcination time is 2～4 hours, and calcining heat and asynchronism(-nization) obtain the tourmaline powder of different colours;
(4) wet ball grinding: will carry out ball milling in the burnt tourmaline powder adding agitating ball mill, add mill and be situated between and grinding aid in ball milling, through screening, mill is situated between and stays in the ball mill ball milling after 36～80 hours, can obtain the tourmaline slip of particle diameter 15～60nm, wherein:
Tourmaline powder and the ratio of grinding Jie: 1: 4～1: 6;
The ratio of tourmaline powder and dispersant water: 1: 1～1: 1.5;
The ratio of tourmaline powder and grinding aid is: 1: 0.005～1: 0.05;
(5) spray-drying: resulting tourmaline slip is dispersed into droplet sprays in the hot blast, moisture content≤1 ‰; Grinding aid decomposes in the time of 300-500 ℃; Through granulation, the tourmaline particle that makes is spherical;
(6) powder is separated reunion: the tourmaline powder that spray-drying is intact joins in the crushing chamber from charging aperture, under the effect of high velocity air, material is by the bump between self particle, air-flow is to the impact of the impact shear effect of material and material and other parts, friction, shearing and make material separate reunion, also play simultaneously certain pulverization, the tourmaline powder particle diameter 15～60nm after secondary gas flow is pulverized;
(7) packaging and storing: with the tourmaline ultrafine powder that processes, pack on request, deposit in dry frescade.
2, nano level superfine tourmaline micropowder preparing process according to claim 1 is characterized in that grinding aid is any one in polyacrylate, salt or the polyacrylamide.
3, nano level superfine tourmaline micropowder preparing process according to claim 1 is characterized in that grinding being situated between and is in zirconia or the aluminium oxide any one.
4, nano level superfine tourmaline micropowder preparing process according to claim 3, the particle diameter that it is characterized in that grinding Jie is 2～5mm.
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|---|---|---|---|
| CN 200410000816 CN1265887C (en) | 2004-01-17 | 2004-01-17 | Method for preparing nanometer ultra-fine tourmaline powder |
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|---|---|---|---|
| CN 200410000816 CN1265887C (en) | 2004-01-17 | 2004-01-17 | Method for preparing nanometer ultra-fine tourmaline powder |
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| CN1265887C true CN1265887C (en) | 2006-07-26 |
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| CN 200410000816 Expired - Fee Related CN1265887C (en) | 2004-01-17 | 2004-01-17 | Method for preparing nanometer ultra-fine tourmaline powder |
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| CN102558939A (en) * | 2011-12-30 | 2012-07-11 | 长沙科星纳米工程技术有限公司 | Method for preparing new nano-cuprous oxide antifouling material by mechanochemical method |
| CN103920574B (en) * | 2013-01-11 | 2017-04-26 | 张仁鸿 | Method for micronization of material having human body far-infrared ray wave band |
| CN103466645B (en) * | 2013-09-27 | 2015-05-20 | 上海冠旗电子新材料股份有限公司 | Method for preparing nano-silica by wet grinding |
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| CN106380897A (en) * | 2016-08-20 | 2017-02-08 | 谢裕梦 | A method of preparing ultrafine tourmaline powder |
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| CN107096610B (en) * | 2017-05-13 | 2019-01-01 | 河北工业大学 | A method of preparing nano-scale tourmaline powder |
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| CN110484204B (en) * | 2019-09-05 | 2022-10-04 | 北京工业职业技术学院 | Preparation method of high-whiteness negative ion powder |
| CN110981501A (en) * | 2019-12-27 | 2020-04-10 | 中能普发科技江苏有限公司 | Preparation device and process of high-purity nano ceramic material |
| CN111820242A (en) * | 2020-07-27 | 2020-10-27 | 安徽国微华芯环境科技有限公司 | Preparation process and application of antibacterial and odor-removing granules |
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