CN1598081A - Technology for continuous producing four-feet shape zine oxide whisker and rotating furnace thereof - Google Patents
Technology for continuous producing four-feet shape zine oxide whisker and rotating furnace thereof Download PDFInfo
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- CN1598081A CN1598081A CN 200410050238 CN200410050238A CN1598081A CN 1598081 A CN1598081 A CN 1598081A CN 200410050238 CN200410050238 CN 200410050238 CN 200410050238 A CN200410050238 A CN 200410050238A CN 1598081 A CN1598081 A CN 1598081A
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- whisker
- zinc oxide
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- clay
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- 238000005516 engineering process Methods 0.000 title claims abstract description 8
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 54
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000013078 crystal Substances 0.000 claims abstract description 29
- 239000011787 zinc oxide Substances 0.000 claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 21
- 239000004927 clay Substances 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 10
- 230000032683 aging Effects 0.000 claims abstract description 4
- 229910052751 metal Inorganic materials 0.000 claims description 15
- 239000002184 metal Substances 0.000 claims description 15
- 229910052725 zinc Inorganic materials 0.000 claims description 15
- 239000011701 zinc Substances 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 238000010924 continuous production Methods 0.000 claims description 12
- 239000002994 raw material Substances 0.000 claims description 11
- 238000000227 grinding Methods 0.000 claims description 7
- 239000003054 catalyst Substances 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 239000002689 soil Substances 0.000 claims description 5
- 150000002978 peroxides Chemical class 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 3
- 238000012216 screening Methods 0.000 claims description 3
- 206010013786 Dry skin Diseases 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 238000005485 electric heating Methods 0.000 claims description 2
- 230000005611 electricity Effects 0.000 claims description 2
- 238000011049 filling Methods 0.000 claims description 2
- 238000002309 gasification Methods 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 5
- 150000001875 compounds Chemical class 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 230000005540 biological transmission Effects 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 229920000742 Cotton Polymers 0.000 description 4
- 238000009825 accumulation Methods 0.000 description 4
- 230000035807 sensation Effects 0.000 description 4
- 230000000007 visual effect Effects 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000003517 fume Substances 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000003082 abrasive agent Substances 0.000 description 2
- 239000011358 absorbing material Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000013016 damping Methods 0.000 description 2
- AFZSMODLJJCVPP-UHFFFAOYSA-N dibenzothiazol-2-yl disulfide Chemical compound C1=CC=C2SC(SSC=3SC4=CC=CC=C4N=3)=NC2=C1 AFZSMODLJJCVPP-UHFFFAOYSA-N 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 230000005622 photoelectricity Effects 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 238000002203 pretreatment Methods 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- 229910052984 zinc sulfide Inorganic materials 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- HPNSNYBUADCFDR-UHFFFAOYSA-N chromafenozide Chemical compound CC1=CC(C)=CC(C(=O)N(NC(=O)C=2C(=C3CCCOC3=CC=2)C)C(C)(C)C)=C1 HPNSNYBUADCFDR-UHFFFAOYSA-N 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000012745 toughening agent Substances 0.000 description 1
- RNWHGQJWIACOKP-UHFFFAOYSA-N zinc;oxygen(2-) Chemical group [O-2].[Zn+2] RNWHGQJWIACOKP-UHFFFAOYSA-N 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
This invention relates to a four-foot zinc oxide crystal whisker continuous generation technology and its revolver. The mixed aging zinc powder and growth substance-clay is putted onto the rotary reaction tray from the feed port of the crystal whisker continuous revolver. The zinc powder in the compound turns into four-foot zinc oxide crystal whisker in the hot atmosphyere of 800-1000 deg.C. The four-foot zinc oxide crystal whisker which is equal style, high purity, the yield is more than 95%, and this method realized the continuation of the preparation of four-foot zinc oxide crystal whisker and its industrial production.
Description
Technical field
The present invention relates to a kind of preparation and equipment thereof of novel material, particularly a kind of four-leg crystal whisker of zinc oxide continuous production processes and rotary oven.
Background technology
This whisker has a wide range of applications as the additive of matrix material, can be used as the toughener of materials such as metal, pottery, macromolecule resin, also can be used for sound insulation, damping material, filtering material, support of the catalyst, gas sensor, electromagnetic shielding material, absorbing material, high-abrasive material etc., also can be used for different field such as photoelectricity, electronic component, thiofide, coating, printing ink, pigment, makeup.
Japanese Matsushita Electric Industrial Industry Co., Ltd discloses a kind of preparation technology and continuous production device of ZnOw in US5158643 (1989); its core is the preoxidation of zinc powder mechanochemistry, protection of inert gas and fluidized roaster, realizes what serialization was produced.This method is comparatively complicated, and regularity is poor, yield is low.CN1224777A then adopts the mode of two reaction boxs exchanges to realize serialization production, and it reduces in the stove amount of oxygen by the principle that when gases are heated, they expand and controls whisker growth, and its essence is still batch production; And atmosphere control randomness is strong, is difficult to guarantee the whisker normal growth.The mode that CN1321798A describes a kind of band shape or ring-form calcining furnace realizes serialization production.Core is blast volume and the control of eolian branch that reaction atmosphere passes through certain position in the stove, and material with the truck tangential movement, at discharge end, is sucked out chilling in stove, separate whisker and non-crystal whisker products and unreacted material in cyclonic separator, and get crystal whisker products.This method is still comparatively complicated, and the control difficulty is big, and four-leg crystal whisker of zinc oxide yield and regularity are undesirable.
Summary of the invention
The object of the present invention is to provide a kind of four-leg crystal whisker of zinc oxide continuous production processes and rotary oven production equipment, its prepared four-leg crystal whisker of zinc oxide form size evenly, purity is high, yield is high, and method is simple, the production efficiency height, can realize the big production of serialization industry.
The objective of the invention is to be achieved through the following technical solutions:
The four-leg crystal whisker of zinc oxide continuous production processes, with the clay is growth catalyst, the mixing raw material of the ageing metal zinc that is pre-mixed and the growth catalyst-clay charging opening from whisker continuous production rotary oven is joined on the revolving reaction pallet, and the zinc powder in the revolving reaction pallet in the mixing raw material generates four-leg crystal whisker of zinc oxide in 800～1100 ℃ of warm air atmosphere.Metal zinc and clay part by weight are 1: 0.1～1: 10.The particle diameter of metal zinc and clay is less than 0.3mm.Metal zinc is preoxidation; Be metal zinc in deionized water, by 10～60 fens kinds of ball mill grinding, pour into then in pallet, can add a little peroxide water H
2O
2Leave standstill-ageing is preoxidation 8～72 hours, outwells the water in the pallet again, 50～100 ℃ of dryings again.Clay is the common soil in the farmland that does not contain sandstone; Common soil passes through oven dry, grinding, screening, 100～500 ℃ of processing of high temperature, grinds, sieves and prepare.Four-leg crystal whisker of zinc oxide continuous production rotary oven is the energy with the electricity, by carbon-point or electric heating piece heat supply, four parts-Jia raw material part, zinc powder gasification and whisker growth part, whisker output section and residue output section are divided in the internal space; Rotary oven is a semi closed, and a charging opening, compressed air inlet, whisker discharge port and residue discharge port are arranged; The revolving reaction pallet drives material movement; 3～20 minutes/circle of its speed of rotation prepares required time according to whisker and determines.Feed rate is controlled by the end mouth of filling tube and distance and the speed of rotation between the revolving reaction pallet.
Description of drawings:
Fig. 1 is the continuous production rotary oven structural representation of high-regularity four-leg crystal whisker of zinc oxide of the present invention;
Fig. 2 is the stereoscan photograph (SEM) of the four-leg crystal whisker of zinc oxide of preparation among the embodiment 1, and its sample carried out the vacuum metal spraying to be handled;
Fig. 3 is the X-ray diffraction spectra of the four-leg crystal whisker of zinc oxide of preparation among the embodiment 1.
Embodiment
Technological line of the present invention be with metal zinc in deionized water, by ball mill grinding 10～60 minutes, pour into then in pallet and (can add a little peroxide water H
2O
2) still aging (preoxidation) 8～72 hours, outwell the water in the pallet again, dry again.The mixing raw material of the metal zinc that will be pre-mixed and growth catalyst-clay joins revolving reaction pallet (1) from the feeder (10) (end mouth of charging opening and distance and the feed rate that speed of rotation is controlled between the revolving reaction pallet) of whisker quantity-produced rotary oven then, the zinc powder of mixing raw material is gasificated into zinc fume in 800～1100 ℃ of warm air atmosphere in the revolving reaction pallet, zinc fume and pressurized air meet, and oxidation generates four-leg crystal whisker of zinc oxide.When the product (four-leg crystal whisker of zinc oxide) that reaction generates runs into whisker stripper (4) in the reaction pallet, the four-leg crystal whisker of zinc oxide on upper strata is scraped from whisker outlet (12) by the whisker stripper and separates, collect, the bottom residue is then discharged from residue outlet (13) by residue evideur (5).
These method characteristics are effectively to control the growth conditions that zinc fume and oxygen partial pressure satisfy four-leg crystal whisker of zinc oxide by control feed rate, air supply and growth catalyst, make the zinc powder total overall reaction generate ZnOw, and well grow into the high-regularity whisker.
This zinc powder is a raw material, and purity is not done particular requirement, and general commercially available prod gets final product.109 ° of every pins of the angle of any two pins of whisker are about 40～60 μ m, and base diameter is 2.0～3.0 μ m, and length-to-diameter ratio is 20～30.The X-ray diffraction spectra proves that this whisker has the hexagonal system wurtzite crystal structure, and is the ZnOw of based on very high purity.
Can prepare high-purity, uniform four-leg crystal whisker of zinc oxide easily with processing method described in the invention.It is remarkable that this whisker is used for metal matrix, polymer-based, ceramic matric composite strengthens toughening effect, and give material with isotropy.Also can be used for sound insulation damping material, filtering material, support of the catalyst, gas sensor, electromagnetic shielding material, absorbing material, high-abrasive material etc., also can be used for different field such as photoelectricity, electronic component, thiofide, coating, printing ink, pigment, makeup, have a wide range of applications.
(1) revolving reaction pallet among the figure; (2) adiabatic pallet; (3) newel; (4) whisker stripper; (5) residue evideur; (6) residue baffle plate; (7) furnace body outer wall; (8) body of heater top cover; (9) body of heater bearing; (10) feeder; (11) feeder top cover; (12) whisker outlet; (13) residue outlet; (14) compressed air inlet; (15) baffle plate of charging opening.
Rotary oven specifies as follows:
Oven body part is supported by body of heater bearing (9), and body of heater is connected by the adiabatic pallet (2) in the body of heater bearing with the body of heater bearing, and transmission mechanism is fixed on the transmission shaft, and transmission mechanism driven rotary reaction pallet (1) rotates.Transmission mechanism and revolving reaction pallet (1) are separated by adiabatic pallet (2), avoid the works better of temperatures involved transmission mechanism.Also be fixed with whisker stripper (4), residue evideur (5) and residue baffle plate (6) on the newel (3), and be installed in the body of heater.Feeding section is made up of feeder (10) and feeder top cover (11), and the feeding section oblique cutting is on body of heater.Body of heater is made up of furnace body outer wall (7) and body of heater top cover (8) two portions.
Embodiment 1
With 1 kilogram of commercially available zinc powder in deionized water with ball mill grinding 10 minutes, the soaking at room temperature that (adds several peroxide water) then in deionized water 24 hours is separated zinc powder and deionized water, dry zinc powder.
With do not contain common soil in the farmland of sandstone through oven dry, grinding, screening, pyroprocessing (100～500 ℃), grind again, sieve and obtain the pre-treatment good clay growth catalyst of particle diameter less than 0.3mm.
Zinc powder that pre-treatment is good and clay are even by 1: 0.5 mixed, are fed in the feeder of rotary oven.Rotary oven is preheating to 940 ℃, and compressed air require is transferred to 400ml/min.Opened rotary oven turn switch control revolution 6 minutes/change, open the baffle plate of the charging opening of feeder, raw material begins to enter into the revolving reaction pallet of rotary oven, constantly enter in the rotary oven with pallet rotation raw material, four-leg crystal whisker of zinc oxide comes out to fall into the whisker collection container from the whisker discharge port, and residue falls into the residue collection container from the residue outlet.
Whisker amount by zinc powder add-on and collection is calculated, and the whisker yield is 98%.Its outward appearance loose cotton-wool shape accumulation body that is white in color, proportion 0.04～0.10g/cm
3, press flexible on time sensation.Observe whisker growth good (no diauxie) from SEM (Fig. 2), be four regular pin shape whiskers of homogeneous, non-four pin shape whiskers such as no platelet or tripod, five pin and six pin, and the whisker size is evenly.By ten visual field calculating mean values, four pin shape whisker regularities are 99%.Every pin of whisker is about 45～55 μ m, and base diameter is 2.0～3.0 μ m, 109 ° of any two pin angles.The X-ray diffraction spectra of Fig. 3 proves that this whisker has the hexagonal system wurtzite crystal structure, and is the ZnOw of based on very high purity.
Press embodiment 1, only change zinc powder and clay and be 1: 10 ratio.Whisker amount by zinc powder add-on and collection is calculated, and the whisker yield is 98%.Its outward appearance loose cotton-wool shape accumulation body that is white in color, proportion 0.04～0.10g/cm
3, press flexible on time sensation.The observation whisker growth is better, and the whisker of diauxic growth is 5 ‰, is four regular pin shape whiskers of homogeneous, non-four pin shape whiskers such as no platelet or tripod, five pin and six pin, and the whisker size is evenly.By ten visual field calculating mean values, four pin shape whisker regularities are 98%.Every pin of whisker is about 40～60 μ m, and base diameter is 2.0～3.0 μ m, 109 ° of any two pin angles.
Press embodiment 1, change zinc powder and clay are 1: 0.1 ratio, change compressed air require to 600ml/min.Whisker amount by zinc powder add-on and collection is calculated, and the whisker yield is 96%.Its outward appearance loose cotton-wool shape accumulation body that is white in color, proportion 0.04～0.10g/cm
3, press flexible on time sensation.The observation whisker growth is better, and the whisker of diauxic growth is 3 ‰, is four regular pin shape whiskers of homogeneous, non-four pin shape whiskers such as no platelet or tripod, five pin and six pin, and the whisker size is evenly.By ten visual field calculating mean values, four pin shape whisker regularities are 98%.Every pin of whisker is about 40～60 μ m, and base diameter is 2.0～3.0 μ m, 109 ° of any two pin angles.
Embodiment 4
Press embodiment 1, only change 20 minutes/commentaries on classics of rotary oven rotation revolution.Whisker amount by zinc powder add-on and collection is calculated, and the whisker yield is 98.5%.Its outward appearance loose cotton-wool shape accumulation body that is white in color, proportion 0.04～0.10g/cm
3, press flexible on time sensation.Observe whisker growth good (no diauxie), be four regular pin shape whiskers of homogeneous, non-four pin shape whiskers such as no platelet or tripod, five pin and six pin, and the whisker size is evenly.By ten visual field calculating mean values, four pin shape whisker regularities are 99%.Every pin of whisker is about 45～55 μ m, and base diameter is 2.0～3.0 μ m, 109 ° of any two pin angles.
Claims (7)
1. four-leg crystal whisker of zinc oxide continuous production processes, it is characterized in that: be growth catalyst with the clay, the mixing raw material of the ageing metal zinc that is pre-mixed and the growth catalyst-clay charging opening from whisker continuous production rotary oven is joined on the revolving reaction pallet, and the zinc powder in the revolving reaction pallet in the mixing raw material generates four-leg crystal whisker of zinc oxide in 800～1100 ℃ of warm air atmosphere.
2. according to the described continuous zinc oxide whisker producing technology of claim 1, it is characterized in that: metal zinc and clay part by weight are 1: 0.1～1: 10.
3. according to the described continuous zinc oxide whisker producing technology of claim 1, it is characterized in that: the particle diameter of metal zinc and clay is less than 0.3mm.
4. according to the described continuous zinc oxide whisker producing technology of claim 1, it is characterized in that: metal zinc is preoxidation; Be metal zinc in deionized water, by 10～60 fens kinds of ball mill grinding, pour into then in pallet, can add a little peroxide water H
2O
2Leave standstill-ageing is preoxidation 8～72 hours, outwells the water in the pallet again, 50～100 ℃ of dryings again.
5. according to the described continuous zinc oxide whisker producing technology of claim 1, it is characterized in that: clay is the common soil in the farmland that does not contain sandstone; Common soil passes through oven dry, grinding, screening, 100～500 ℃ of processing of high temperature, grinds, sieves and prepare.
6. four-leg crystal whisker of zinc oxide continuous production rotary oven is characterized in that: be the energy with the electricity, by carbon-point or electric heating piece heat supply, four parts-Jia raw material part, zinc powder gasification and whisker growth part, whisker output section and residue output section are divided in the internal space; Rotary oven is a semi closed, and a charging opening, compressed air inlet, whisker discharge port and residue discharge port are arranged; The revolving reaction pallet drives material movement; 3～20 minutes/circle of its speed of rotation prepares required time according to whisker and determines.
7. according to the described ZnOw continuous production of claim 6 rotary oven, it is characterized in that: feed rate is controlled by the end mouth of filling tube and distance and the speed of rotation between the revolving reaction pallet.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100502381A CN1316077C (en) | 2004-08-12 | 2004-08-12 | Technology for continuous producing four-feet shape zine oxide whisker and rotating furnace thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100502381A CN1316077C (en) | 2004-08-12 | 2004-08-12 | Technology for continuous producing four-feet shape zine oxide whisker and rotating furnace thereof |
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| Publication Number | Publication Date |
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| CN1598081A true CN1598081A (en) | 2005-03-23 |
| CN1316077C CN1316077C (en) | 2007-05-16 |
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| CNB2004100502381A Expired - Fee Related CN1316077C (en) | 2004-08-12 | 2004-08-12 | Technology for continuous producing four-feet shape zine oxide whisker and rotating furnace thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1320176C (en) * | 2005-05-08 | 2007-06-06 | 西南交通大学 | Magnetic modified nanometer zinc oxide whiskers and production thereof |
| CN100334265C (en) * | 2005-07-01 | 2007-08-29 | 中南大学 | Process and equipment for continuously producing tetrapod-like zinc oxide whisker |
| CN112853488A (en) * | 2021-01-08 | 2021-05-28 | 四川省又飞新材料有限责任公司 | Equipment and method for preparing tetrapod-like zinc oxide whiskers by using modified montmorillonite catalyst |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1077613C (en) * | 1998-01-24 | 2002-01-09 | 西南交通大学 | Zinc oxide whisker continuous production process and device |
| CN1086211C (en) * | 1999-04-22 | 2002-06-12 | 中国科学院金属研究所 | Process for preparing four-leg crystal whisker of zinc oxide |
| CN1170011C (en) * | 2002-01-18 | 2004-10-06 | 清华大学 | Process for preparing zinc oxide whiskers with different forms by using gasification and oxidation method |
-
2004
- 2004-08-12 CN CNB2004100502381A patent/CN1316077C/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1320176C (en) * | 2005-05-08 | 2007-06-06 | 西南交通大学 | Magnetic modified nanometer zinc oxide whiskers and production thereof |
| CN100334265C (en) * | 2005-07-01 | 2007-08-29 | 中南大学 | Process and equipment for continuously producing tetrapod-like zinc oxide whisker |
| CN112853488A (en) * | 2021-01-08 | 2021-05-28 | 四川省又飞新材料有限责任公司 | Equipment and method for preparing tetrapod-like zinc oxide whiskers by using modified montmorillonite catalyst |
| CN112853488B (en) * | 2021-01-08 | 2024-02-06 | 四川祺又飞新材料科技有限责任公司 | Equipment and method for preparing tetrapod-like zinc oxide whisker by modified montmorillonite catalyst |
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