CN105200519A - Preparation method of sepiolite-tetrapod zinc oxide whisker composite material - Google Patents
Preparation method of sepiolite-tetrapod zinc oxide whisker composite material Download PDFInfo
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- CN105200519A CN105200519A CN201510678218.7A CN201510678218A CN105200519A CN 105200519 A CN105200519 A CN 105200519A CN 201510678218 A CN201510678218 A CN 201510678218A CN 105200519 A CN105200519 A CN 105200519A
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- sepiolite
- zinc oxide
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- crystal whisker
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Abstract
The invention relates to a preparation method of a sepiolite-tetrapod zinc oxide whisker composite material. Sepiolite has very high adsorption performance and good dispersing performance and can be taken as a carrier and a framework of tetrapod zinc oxide whiskers, and respective use performance is not influenced. The preparation method comprises steps as follows: the sepiolite is dissolved in ethanol, methanol or hydrogen peroxide, is stirred uniformly and dried after separation, and sepiolite powder is obtained; the sepiolite powder and zinc powder are mixed, dissolved in distilled water, ethanol, methanol or hydrogen peroxide and stirred and mixed uniformly; a solid mixture obtained after separation is placed in a drying oven for drying; dry powder is placed in a high-temperature stove for calcination treatment, and the sepiolite-tetrapod zinc oxide whisker composite material is obtained. The prepared composite material has performance including wear resistance, strength enhancement, damping performance, slip resistance, nose reduction, ageing resistance, antistatic property, antibacterial property and the like and can be widely applied to materials such as a coating, an antibacterial material, an antistatic material, a wear-reducing and wear-resistant material and the like, the operation technology is simple, and the economic cost-performance ratio is high.
Description
Technical field
The present invention relates to the preparation method of a kind of sepiolite-four acicular type zinc oxide crystal whisker matrix material, belong to field of compound material.
Background technology
Four acicular type zinc oxide crystal whisker has the incomparable premium properties of common zinc oxide, is readily embodied in being uniformly distributed in body material, to improve the physicals of material, gives the functional performance of the multiple uniqueness of material simultaneously.Four acicular type zinc oxide crystal whisker has wear-resisting, enhancing, damping, anti-skidding, noise reduction, the performance such as anti-aging, antistatic, antibacterial, is widely used in multiple field.Mostly adopting with zinc powder is at present that four acicular type zinc oxide crystal whisker prepared by raw material; but in preparation process; the zinc oxide of zinc powder Surface Creation can form coating film; stop the further oxidizing reaction of its inner zinc powder; cause that the four acicular type zinc oxide crystal whisker productive rate that generates is low, purity is not high, have impact on suitability for industrialized production and mass-producing and use.
Sepiolite belongs to rhombic system or oblique system, color-variable, and physique is light, and shrinking percentage is low, and plasticity-is good.Sepiolite is moisture magnesium silicate, and its standard crystal chemical formula is Mg
8(H
2o)
4[Si
6o
16]
2(OH)
48H
2o.Sepiolite has specific surface area maximum in non-metallic minerals and unique internal gutter structure, can adsorb a large amount of water or polar material, comprise low polar material in pore passage structure.Therefore sepiolite has the performances such as extremely strong absorption, decolouring and dispersion.Utilize the pore passage structure of sepiolite uniqueness and extremely strong absorption property, can be used as the carrier and skeleton that generate four acicular type zinc oxide crystal whisker, and the respective use properties of sepiolite and ZnOw is independent of each other.
Summary 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 the preparation method of a kind of sepiolite-four acicular type zinc oxide crystal whisker matrix material.
The technical solution used in the present invention is as follows:
A preparation method for sepiolite-four acicular type zinc oxide crystal whisker matrix material, carries out as follows:
(sepiolite is dissolved in wherein a kind of solution of dehydrated alcohol, anhydrous methanol or 10%-20% hydrogen peroxide by (1), stirs, and filters or carries out drying after centrifugation, obtaining sepiolite powder;
(2) sepiolite powder step (1) obtained and zinc powder mix in the mass parts ratio of 0.01:1 ~ 100:1, are dissolved in distilled water, ethanol, methyl alcohol, hydrogen peroxide wherein in a kind of solution, and normal temperature and pressure stirs 1-2h to mixing;
(3) mixing solutions step (2) obtained after filtration or centrifugal method be separated, the solid mixture obtained is put and carries out drying in an oven, obtain the dried powder of mixture;
(4) High Temperature Furnaces Heating Apparatus dried powder that step (3) obtains being placed in 600 ~ 1200 DEG C carries out calcination processing, obtains sepiolite-four acicular type zinc oxide crystal whisker matrix material.
The technical solution used in the present invention compared with prior art has following advantage:
Sepiolite prepared by the present invention-four acicular type zinc oxide crystal whisker matrix material, there is wear-resisting, enhancing, damping, anti-skidding, noise reduction, the performance such as anti-aging, antistatic, antibacterial, can be widely used in the materials such as coating, anti-biotic material, antistatic material and anti-attrition be wear-resistant.Adopt this preparation method, operating procedure is simple, and economic cost performance is high, can promote that four acicular type zinc oxide crystal whisker suitability for industrialized production and mass-producing use.
Further, prioritization scheme of the present invention:
The middle zinc powder of described step (2) and the sepiolite powder obtained after processing adopt solid-phase ball milling method to be dry mixed, and ball milling speed is 600RPM, and Ball-milling Time is 3-12h.
In described step (3), drying temperature is less than 150 DEG C.
In described step (4), calcining temperature is 600 ~ 1200 DEG C, and calcining at constant temperature 0.1 ~ 3h, calcination atmosphere is air, and control airshed is 0 ~ 1600mL/min.
Embodiment
The detailed description below for specific embodiment, the present invention carried out, but embodiment does not limit in any form the present invention.
Embodiment 1:
A preparation method for sepiolite-four acicular type zinc oxide crystal whisker matrix material, carries out as follows:
(1) getting sepiolite 5g is dissolved in the ethanolic soln of 50mL, and stirring at normal temperature is even, dry after filtering, and obtains sepiolite powder;
(2) get the sepiolite powder 0.1g after process, zinc powder 10g, adopt ball milled, with 600RPM speed ball milling 3h, obtain the powder mixed, be dissolved in 50mL ethanolic soln, under normal temperature and pressure, stir 1h, make it mix;
(3) be separated after filtration by the mixing solutions that step (2) obtains, put by the solid mixture obtained and carry out drying in an oven, drying temperature is 110 DEG C, obtains the powder mixed after drying;
(4) be placed in High Temperature Furnaces Heating Apparatus after the dried powder that step (3) obtains being cooled to room temperature and calcine, calcining temperature is warming up to 600 DEG C gradually by room temperature, calcination atmosphere is air, control airshed is 100mL/min, constant temperature 0.5h after temperature rises to 600 DEG C, the constant reaction product of airshed cools to room temperature taking-up with the furnace afterwards, obtains sepiolite-four acicular type zinc oxide crystal whisker matrix material.
Embodiment 2:
A preparation method for sepiolite-four acicular type zinc oxide crystal whisker matrix material, carries out as follows:
(1) getting sepiolite 5g is dissolved in the ethanolic soln of 50mL, and stirring at normal temperature is even, dry after filtering, and obtains sepiolite powder;
(2) get the sepiolite powder 1g after process, zinc powder 100g, adopt ball milled, with 600RPM speed ball milling 12h, obtain the powder mixed, be dissolved in 1000mL ethanolic soln, under normal temperature and pressure, stir 1h, make it mix;
(3) be separated after filtration by the mixing solutions that step (2) obtains, put by the solid mixture obtained and carry out drying in an oven, drying temperature is 110 DEG C, obtains the powder mixed after drying;
(4) be placed in High Temperature Furnaces Heating Apparatus after the dried powder that step (3) obtains being cooled to room temperature and calcine, calcining temperature is warming up to 1200 DEG C gradually by room temperature, calcination atmosphere is air, control airshed is 500mL/min, constant temperature 3h after temperature rises to 1200 DEG C, the constant reaction product of airshed cools to room temperature taking-up with the furnace afterwards, obtains sepiolite-four acicular type zinc oxide crystal whisker matrix material.
Embodiment 3:
A preparation method for sepiolite-four acicular type zinc oxide crystal whisker matrix material, carries out as follows:
(1) getting sepiolite 5g is dissolved in the ethanolic soln of 50mL, and stirring at normal temperature is even, dry after filtering, and obtains sepiolite powder;
(2) get the sepiolite powder 1g after process, zinc powder 100g, adopt ball milled, with 600RPM speed ball milling 12h, obtain the powder mixed, be dissolved in 1000mL ethanolic soln, under normal temperature and pressure, stir 1h, make it mix;
(3) be separated after filtration by the mixing solutions that step (2) obtains, put by the solid mixture obtained and carry out drying in an oven, drying temperature is 110 DEG C, obtains the powder mixed after drying;
(4) be placed in High Temperature Furnaces Heating Apparatus after the dried powder that step (3) obtains being cooled to room temperature and calcine, calcining temperature is warming up to 1000 DEG C gradually by room temperature, calcination atmosphere is air, control airshed is 1000mL/min, constant temperature 1.5h after temperature rises to 1000 DEG C, the constant reaction product of airshed cools to room temperature taking-up with the furnace afterwards, obtains sepiolite-four acicular type zinc oxide crystal whisker matrix material.
Embodiment 4:
A preparation method for sepiolite-four acicular type zinc oxide crystal whisker matrix material, carries out as follows:
(1) getting sepiolite 70g is dissolved in the ethanolic soln of 700mL, and stirring at normal temperature is even, dry after filtering, and obtains sepiolite powder;
(2) get the sepiolite powder 50g after process, zinc powder 0.5g, adopt ball milled, with 600RPM speed ball milling 7h, obtain the powder mixed, be dissolved in 200mL ethanolic soln, under normal temperature and pressure, stir 1h, make it mix;
(3) be separated after filtration by the mixing solutions that step (2) obtains, put by the solid mixture obtained and carry out drying in an oven, drying temperature is 110 DEG C, obtains the powder mixed after drying;
(4) be placed in High Temperature Furnaces Heating Apparatus after the dried powder that step (3) obtains being cooled to room temperature and calcine, calcining temperature is warming up to 800 DEG C gradually by room temperature, calcination atmosphere is air, control airshed is 1200mL/min, constant temperature 1h after temperature rises to 800 DEG C, the constant reaction product of airshed cools to room temperature taking-up with the furnace afterwards, obtains sepiolite-four acicular type zinc oxide crystal whisker matrix material.
Embodiment 5:
A preparation method for sepiolite-four acicular type zinc oxide crystal whisker matrix material, carries out as follows:
(1) getting sepiolite 120g is dissolved in the ethanolic soln of 1200mL, and stirring at normal temperature is even, dry after filtering, and obtains sepiolite powder;
(2) get the sepiolite powder 100g after process, zinc powder 1g, adopt ball milled, with 600RPM speed ball milling 12h, obtain the powder mixed, be dissolved in 500mL ethanolic soln, under normal temperature and pressure, stir 1h, make it mix;
(3) be separated after filtration by the mixing solutions that step (2) obtains, put by the solid mixture obtained and carry out drying in an oven, drying temperature is 110 DEG C, obtains the powder mixed after drying;
(4) be placed in High Temperature Furnaces Heating Apparatus after the dried powder that step (3) obtains being cooled to room temperature and calcine, calcining temperature is warming up to 1000 DEG C gradually by room temperature, calcination atmosphere is air, control airshed is 1600mL/min, constant temperature 0.2h after temperature rises to 1000 DEG C, the constant reaction product of airshed cools to room temperature taking-up with the furnace afterwards, obtains sepiolite-four acicular type zinc oxide crystal whisker matrix material.
Claims (4)
1. a preparation method for sepiolite-four acicular type zinc oxide crystal whisker matrix material, is characterized in that, carries out as follows:
(1) sepiolite is dissolved in wherein a kind of solution of dehydrated alcohol, anhydrous methanol or 10%-20% hydrogen peroxide, stirs, filter or carry out drying after centrifugation, obtaining sepiolite powder;
(2) sepiolite powder step (1) obtained and zinc powder mix in the mass parts ratio of 0.01:1 ~ 100:1, are dissolved in distilled water, ethanol, methyl alcohol, hydrogen peroxide wherein in a kind of solution, and normal temperature and pressure stirs 1-2h to mixing;
(3) mixing solutions step (2) obtained after filtration or centrifugal method be separated, the solid mixture obtained is put and carries out drying in an oven, obtain the dried powder of mixture;
(4) High Temperature Furnaces Heating Apparatus dried powder that step (3) obtains being placed in 600 ~ 1200 DEG C carries out calcination processing, obtains sepiolite-four acicular type zinc oxide crystal whisker matrix material.
2. the preparation method of sepiolite-four acicular type zinc oxide crystal whisker matrix material according to material requirements 1, it is characterized in that, the middle zinc powder of step (2) and the sepiolite powder obtained after processing adopt solid-phase ball milling method to be dry mixed, and ball milling speed is 600RPM, and Ball-milling Time is 3-12h.
3. the preparation method of sepiolite-four acicular type zinc oxide crystal whisker matrix material according to material requirements 1, is characterized in that, in step (3), drying temperature is less than 150 DEG C.
4. the preparation method of sepiolite-four acicular type zinc oxide crystal whisker matrix material according to material requirements 1, it is characterized in that, in step (4), calcining temperature is 600 ~ 1200 DEG C, calcining at constant temperature 0.1 ~ 3h, calcination atmosphere is air, and control airshed is 0 ~ 1600mL/min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN114836094A (en) * | 2022-05-10 | 2022-08-02 | 浙江华普环保材料有限公司 | Antistatic color-coated sheet |
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|---|---|---|---|---|
| JPH01252600A (en) * | 1987-12-29 | 1989-10-09 | Matsushita Electric Ind Co Ltd | Production of zinc oxide whisker |
| JPH02192499A (en) * | 1989-01-18 | 1990-07-30 | Matsushita Electric Ind Co Ltd | Continuous production of zinc oxide whisker |
| 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 |
-
2015
- 2015-10-20 CN CN201510678218.7A patent/CN105200519B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01252600A (en) * | 1987-12-29 | 1989-10-09 | Matsushita Electric Ind Co Ltd | Production of zinc oxide whisker |
| JPH02192499A (en) * | 1989-01-18 | 1990-07-30 | Matsushita Electric Ind Co Ltd | Continuous production of zinc oxide whisker |
| 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 |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN114836094A (en) * | 2022-05-10 | 2022-08-02 | 浙江华普环保材料有限公司 | Antistatic color-coated sheet |
| 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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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. |