CN105200519B - The preparation method of sepiolite four acicular type zinc oxide crystal whisker composite - Google Patents
The preparation method of sepiolite four acicular type zinc oxide crystal whisker composite Download PDFInfo
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- CN105200519B CN105200519B CN201510678218.7A CN201510678218A CN105200519B CN 105200519 B CN105200519 B CN 105200519B CN 201510678218 A CN201510678218 A CN 201510678218A CN 105200519 B CN105200519 B CN 105200519B
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Abstract
The present invention relates to a kind of preparation method of sepiolite four acicular type zinc oxide crystal whisker composite.Sepiolite has extremely strong absorption property and good dispersive property, in the present invention can as four acicular type zinc oxide crystal whisker carrier and skeleton, and each performance be independent of each other.Preparation method is as follows：Sepiolite is dissolved in ethanol, methanol or hydrogen peroxide, stirred, is dried after separation, sepiolite powder is obtained；With zinc powder mixing, it is dissolved in distilled water, ethanol, methanol, hydrogen peroxide, is uniformly mixed；Put and be dried in an oven through separating solid mixture；Dried powder is placed in high temperature furnace and carries out calcination processing, sepiolite four acicular type zinc oxide crystal whisker composite is obtained.This composite prepared by the present invention has the performances such as wear-resisting, enhancing, damping, anti-skidding, noise reduction, anti-aging, antistatic, antibacterial, it can be widely used in coating, anti-biotic material, anti-static material and the material such as anti-attrition is wear-resistant, operating procedure is simple, and economic cost performance is high.
Description
Technical field
The present invention relates to a kind of preparation method of sepiolite-four acicular type zinc oxide crystal whisker composite, belong to composite
Field.
Background technology
Four acicular type zinc oxide crystal whisker has the incomparable premium properties of common zinc oxide, it is easy to realize in matrix material
In be uniformly distributed, to improve the physical property of material, at the same assign a variety of unique functional characteristics of material.Four-needle-like zinc oxide
Whisker has the performances such as wear-resisting, enhancing, damping, anti-skidding, noise reduction, anti-aging, antistatic, antibacterial, using wide in multiple fields
It is general.Use mostly at present and four acicular type zinc oxide crystal whisker is prepared by raw material of zinc powder, but in preparation process, zinc powder Surface Creation
Zinc oxide can form coating film, prevent its further oxidation reaction of internal zinc powder, cause the four acicular type zinc oxide crystal whisker of generation
Low yield, purity is not high, have impact on industrialized production and scale is used.
Sepiolite belongs to orthorhombic system or monoclinic system, and color-variable, constitution is light, and shrinkage factor is low, and plasticity is good.Sepiolite is
Aqueous magnesium silicate, its standard crystal chemical formula is Mg8(H2O)4[Si6O16]2(OH)4·8H2O.Sepiolite has nonmetallic
Maximum specific surface area and unique internal gutter structure, can adsorb substantial amounts of water or polar material in pore passage structure in mineral
Matter, including low polar substances.Therefore sepiolite has extremely strong absorption, decolourized and the performance such as scattered.Unique using sepiolite
Pore passage structure and extremely strong absorption property, can as generation four acicular type zinc oxide crystal whisker carrier and skeleton, and sepiolite and
The respective performance of ZnOw is independent of each other.
The content of the invention
For preparing the problems such as four acicular type zinc oxide crystal whisker efficiency is low, purity is not high with zinc powder, the present invention discloses a kind of sea
The preparation method of afrodite-four acicular type zinc oxide crystal whisker composite.
The technical solution adopted by the present invention is as follows：
A kind of preparation method of sepiolite-four acicular type zinc oxide crystal whisker composite, is carried out as follows：
（（1）Sepiolite is dissolved in the one of which solution of absolute ethyl alcohol, absolute methanol or 10%-20% hydrogen peroxide, stirred
Mix uniform, be dried after filtering or centrifugation, obtain sepiolite powder；
（2）By step（1）Obtained sepiolite powder and zinc powder is by 0.01:1~100:1 mass parts ratio is well mixed, molten
In distilled water, ethanol, methanol, hydrogen peroxide one of which solution, normal temperature and pressure stirs 1-2h to well mixed；
（3）By step（2）Obtained mixed solution is separated through filtering or centrifugal method, and obtained solid is mixed
Thing is put to be dried in an oven, obtains the dried powder of mixture；
（4）By step（3）Obtained dried powder, which is placed in 600 ~ 1200 DEG C of high temperature furnace, carries out calcination processing, obtains sea
Afrodite-four acicular type zinc oxide crystal whisker composite.
The technical solution adopted by the present invention has the advantage that compared with prior art：
Sepiolite prepared by the present invention-four acicular type zinc oxide crystal whisker composite, with wear-resisting, enhancing, damping, it is anti-skidding,
The performance such as noise reduction, anti-aging, antistatic, antibacterial, can be widely applied to coating, anti-biotic material, anti-static material and anti-attrition wear-resistant
Deng in material.Using this preparation method, operating procedure is simple, and economic cost performance is high, can promote four acicular type zinc oxide crystal whisker
Industrialized production and scale are used.
Further, prioritization scheme of the invention：
The step（2）The sepiolite powder obtained after middle zinc powder and processing carries out dry-mixed, ball milling speed using solid-phase ball milling method
Spend for 600RPM, Ball-milling Time is 3-12h.
The step（3）Middle drying temperature is less than 150 DEG C.
The step（4）Middle calcining heat is 600 ~ 1200 DEG C, and 0.1 ~ 3h of calcining at constant temperature, calcination atmosphere is air, control
Throughput is 0 ~ 1600mL/min.
Embodiment
The detailed description carried out below for specific embodiment to the present invention, but embodiment does not do any type of to the present invention
Limit.
Embodiment 1：
A kind of preparation method of sepiolite-four acicular type zinc oxide crystal whisker composite, is carried out as follows：
（1）Take sepiolite 5g to be dissolved in 50mL ethanol solution, stirring at normal temperature is uniform, dried after filtering, obtain sepiolite
Powder；
（2）Sepiolite powder 0.1g, the zinc powder 10g after processing are taken, using ball-milling method, with 600RPM speed ball milling 3h, is obtained
The powder of mixing, is dissolved in 50mL ethanol solutions, and 1h is stirred under normal temperature and pressure, is well mixed it；
（3）By step（2）Obtained mixed solution is separated through filtering, and the solid mixture obtained is put to enter in an oven
Row drying, drying temperature is 110 DEG C, and well mixed powder is obtained after drying；
（4）By step（3）Obtained dried powder is cooled to be placed in high temperature furnace after room temperature and calcined, calcining heat by
Room temperature is gradually heating to 600 DEG C, and calcination atmosphere is air, and it is 100mL/min to control throughput, and temperature rises to constant temperature after 600 DEG C
0.5h, afterwards the constant reaction product of throughput cool to the furnace room temperature taking-up, obtain sepiolite-four acicular type zinc oxide crystal whisker be combined
Material.
Embodiment 2：
A kind of preparation method of sepiolite-four acicular type zinc oxide crystal whisker composite, is carried out as follows：
（1）Take sepiolite 5g to be dissolved in 50mL ethanol solution, stirring at normal temperature is uniform, dried after filtering, obtain sepiolite
Powder；
（2）Sepiolite powder 1g, the zinc powder 100g after processing are taken, using ball-milling method, with 600RPM speed ball milling 12h, is obtained
The powder of mixing, is dissolved in 1000mL ethanol solutions, and 1h is stirred under normal temperature and pressure, is well mixed it；
（3）By step（2）Obtained mixed solution is separated through filtering, and the solid mixture obtained is put to enter in an oven
Row drying, drying temperature is 110 DEG C, and well mixed powder is obtained after drying；
（4）By step（3）Obtained dried powder is cooled to be placed in high temperature furnace after room temperature and calcined, calcining heat by
Room temperature is gradually heating to 1200 DEG C, and calcination atmosphere is air, and it is 500mL/min to control throughput, and temperature rises to permanent after 1200 DEG C
Warm 3h, afterwards the constant reaction product of throughput cool to the furnace room temperature taking-up, obtain sepiolite-four acicular type zinc oxide crystal whisker be combined
Material.
Embodiment 3：
A kind of preparation method of sepiolite-four acicular type zinc oxide crystal whisker composite, is carried out as follows：
（1）Take sepiolite 5g to be dissolved in 50mL ethanol solution, stirring at normal temperature is uniform, dried after filtering, obtain sepiolite
Powder；
（2）Sepiolite powder 1g, the zinc powder 100g after processing are taken, using ball-milling method, with 600RPM speed ball milling 12h, is obtained
The powder of mixing, is dissolved in 1000mL ethanol solutions, and 1h is stirred under normal temperature and pressure, is well mixed it；
（3）By step（2）Obtained mixed solution is separated through filtering, and the solid mixture obtained is put to enter in an oven
Row drying, drying temperature is 110 DEG C, and well mixed powder is obtained after drying；
（4）By step（3）Obtained dried powder is cooled to be placed in high temperature furnace after room temperature and calcined, calcining heat by
Room temperature is gradually heating to 1000 DEG C, and calcination atmosphere is air, and it is 1000mL/min to control throughput, and temperature rises to permanent after 1000 DEG C
Warm 1.5h, afterwards the constant reaction product of throughput cool to the furnace room temperature taking-up, obtain sepiolite-four acicular type zinc oxide crystal whisker multiple
Condensation material.
Embodiment 4：
A kind of preparation method of sepiolite-four acicular type zinc oxide crystal whisker composite, is carried out as follows：
（1）Take sepiolite 70g to be dissolved in 700mL ethanol solution, stirring at normal temperature is uniform, dried after filtering, obtain Hai Pao
Stone flour；
（2）Sepiolite powder 50g, the zinc powder 0.5g after processing are taken, using ball-milling method, with 600RPM speed ball milling 7h, is obtained
The powder of mixing, is dissolved in 200mL ethanol solutions, and 1h is stirred under normal temperature and pressure, is well mixed it；
（3）By step（2）Obtained mixed solution is separated through filtering, and the solid mixture obtained is put to enter in an oven
Row drying, drying temperature is 110 DEG C, and well mixed powder is obtained after drying；
（4）By step（3）Obtained dried powder is cooled to be placed in high temperature furnace after room temperature and calcined, calcining heat by
Room temperature is gradually heating to 800 DEG C, and calcination atmosphere is air, and it is 1200mL/min to control throughput, and temperature rises to constant temperature after 800 DEG C
1h, afterwards the constant reaction product of throughput cool to the furnace room temperature taking-up, obtain sepiolite-four acicular type zinc oxide crystal whisker composite wood
Material.
Embodiment 5：
A kind of preparation method of sepiolite-four acicular type zinc oxide crystal whisker composite, is carried out as follows：
（1）Take sepiolite 120g to be dissolved in 1200mL ethanol solution, stirring at normal temperature is uniform, dried after filtering, obtain sea
Afrodite powder；
（2）Sepiolite powder 100g, the zinc powder 1g after processing are taken, using ball-milling method, with 600RPM speed ball milling 12h, is obtained
The powder of mixing, is dissolved in 500mL ethanol solutions, and 1h is stirred under normal temperature and pressure, is well mixed it；
（3）By step（2）Obtained mixed solution is separated through filtering, and the solid mixture obtained is put to enter in an oven
Row drying, drying temperature is 110 DEG C, and well mixed powder is obtained after drying；
（4）By step（3）Obtained dried powder is cooled to be placed in high temperature furnace after room temperature and calcined, calcining heat by
Room temperature is gradually heating to 1000 DEG C, and calcination atmosphere is air, and it is 1600mL/min to control throughput, and temperature rises to permanent after 1000 DEG C
Warm 0.2h, afterwards the constant reaction product of throughput cool to the furnace room temperature taking-up, obtain sepiolite-four acicular type zinc oxide crystal whisker multiple
Condensation material.
Claims (1)
1. the preparation method of a kind of sepiolite-four acicular type zinc oxide crystal whisker composite, it is characterised in that enter as follows
OK：
（1）Sepiolite is dissolved in the one of which solution of absolute ethyl alcohol, absolute methanol or 10%-20% hydrogen peroxide, stirring is equal
It is even, it is dried after filtering or centrifugation, obtains sepiolite powder；
（2）By step（1）Obtained sepiolite powder and zinc powder is by 0.01:1~100:1 mass parts ratio is well mixed, using solid
The progress of phase ball-milling method is dry-mixed, and ball milling speed is 600 rpm, and Ball-milling Time is 3-12h；It is dissolved in distilled water, ethanol, methanol, dioxygen
In water one of which solution, normal temperature and pressure stirs 1-2h to well mixed；
（3）By step（2）Obtained mixed solution is separated through filtering or centrifugal method, and obtained solid mixture is put
It is dried in an oven, drying temperature is less than 150 DEG C, obtains the dried powder of mixture；
（4）By step（3）Obtained dried powder, which is placed in 600 ~ 1200 DEG C of high temperature furnace, carries out calcination processing, and calcining heat is
600 ~ 1200 DEG C, 0.1 ~ 3h of calcining at constant temperature, calcination atmosphere is air, control throughput be 0 ~ 1600mL/min, obtain sepiolite-
Four acicular type zinc oxide crystal whisker composite.
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| CN108929656A (en) * | 2018-09-05 | 2018-12-04 | 上海世卿防滑防护科技有限公司 | A kind of ground anti-skid preparation |
| CN114836094B (en) * | 2022-05-10 | 2022-12-06 | 浙江华普环保材料有限公司 | Antistatic color-coated sheet |
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| CN1101952A (en) * | 1994-07-05 | 1995-04-26 | 西南交通大学 | Process for controlling zinc oxide crystal whisker growth by carbon reducer |
| CN1843935A (en) * | 2006-05-15 | 2006-10-11 | 中国科学院上海硅酸盐研究所 | A tetrapod-like nanorod of zinc oxide, its preparation method and apparatus |
| CN1858001A (en) * | 2005-04-29 | 2006-11-08 | 南京大学 | Method for preparing different shape zinc oxide by vacuum limit oxygen method |
| CN101003910A (en) * | 2006-12-15 | 2007-07-25 | 付敏恭 | Zn0 crystallite material, and preparation method |
| CN102659172A (en) * | 2012-04-28 | 2012-09-12 | 江苏科技大学 | Method for preparing nano zinc oxide by vacuum oxygen limiting method |
| CN103950914A (en) * | 2014-04-04 | 2014-07-30 | 西安理工大学 | Preparation method of conductive carbon material with graphene-like structure |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2600762B2 (en) * | 1987-12-29 | 1997-04-16 | 松下電器産業株式会社 | Method for producing zinc oxide whiskers |
| JPH02192499A (en) * | 1989-01-18 | 1990-07-30 | Matsushita Electric Ind Co Ltd | Continuous production of zinc oxide whisker |
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2015
- 2015-10-20 CN CN201510678218.7A patent/CN105200519B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1101952A (en) * | 1994-07-05 | 1995-04-26 | 西南交通大学 | Process for controlling zinc oxide crystal whisker growth by carbon reducer |
| CN1858001A (en) * | 2005-04-29 | 2006-11-08 | 南京大学 | Method for preparing different shape zinc oxide by vacuum limit oxygen method |
| CN1843935A (en) * | 2006-05-15 | 2006-10-11 | 中国科学院上海硅酸盐研究所 | A tetrapod-like nanorod of zinc oxide, its preparation method and apparatus |
| CN101003910A (en) * | 2006-12-15 | 2007-07-25 | 付敏恭 | Zn0 crystallite material, and preparation method |
| CN102659172A (en) * | 2012-04-28 | 2012-09-12 | 江苏科技大学 | Method for preparing nano zinc oxide by vacuum oxygen limiting method |
| CN103950914A (en) * | 2014-04-04 | 2014-07-30 | 西安理工大学 | Preparation method of conductive carbon material with graphene-like structure |
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Effective date of registration: 20201218 Address after: 063020 No.106 Longhua Road, high tech Zone, Tangshan City, Hebei Province Patentee after: Tangshan solang Technology Co.,Ltd. Address before: 063000 No.15 Minzu Road, Caofeidian Industrial Zone, Caofeidian District, Tangshan City, Hebei Province Patentee before: TANGSHAN JIANHUA TECHNOLOGY DEVELOPMENT Co.,Ltd. |