CN108003665A - A kind of surface modifying method of nano-ceramic powder - Google Patents
A kind of surface modifying method of nano-ceramic powder Download PDFInfo
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- CN108003665A CN108003665A CN201711398726.5A CN201711398726A CN108003665A CN 108003665 A CN108003665 A CN 108003665A CN 201711398726 A CN201711398726 A CN 201711398726A CN 108003665 A CN108003665 A CN 108003665A
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- ceramic powder
- surface modifying
- modifying method
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/40—Compounds of aluminium
- C09C1/42—Clays
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/10—Treatment with macromolecular organic compounds
Abstract
The invention discloses a kind of surface modifying method of nano-ceramic powder, include the following steps:(1)Surface activation process,(2)Modification liquid preparation,(3)Surface modification treatment,(4)Drying process.The present invention has carried out special modification to the surface of nano-ceramic powder, effectively improve the surface-active of nano-ceramic powder, improve its dispersing uniformity and respond in coating, enhance the effect that its filling uses, and then the quality of coating is improved, have good value for applications.
Description
Technical field
The invention belongs to ceramic processing techniques field, and in particular to a kind of surface modifying method of nano-ceramic powder.
Background technology
Nano-ceramic powder is that have nanometer scale between solid and molecule(0.1~100nm)Size it is metastable
State intermediate material.With the fine of powder, its Electronic Structure and crystal structure change, and generate bulk material institute
The special effect not having.Well use characteristic since nano-ceramic powder has, and be widely used in building, coating,
The fields such as composite material.In order to improve the use quality of coating, nano-ceramic powder is introduced and added by people, and is achieved certain
Effect, but because nano ceramics powder particles are small, easy reunion, cause dispersion effect bad, it is corresponding for qualities such as the mechanics of coating
Improvement still have large improvement space, this people can be carried out with surface modification treatment when its filling uses, it is most common just
It is to carry out surface coupling modifier processing with silane coupling agent, although the filling for improving nano-ceramic powder uses quality, with
The continuous lifting that people require for coating property, conventional surface modifying treatment can not meet the need that design uses
Ask.
The content of the invention
The purpose of the present invention is for it is existing the problem of, there is provided a kind of surface modifying method of nano-ceramic powder.
The present invention is achieved by the following technical solutions:
A kind of surface modifying method of nano-ceramic powder, includes the following steps:
(1)Surface activation process:
Nano-ceramic powder is put into phosphoric acid solution, is filtered out after 6 ~ 8min of immersion treatment, then puts it into ultraviolet spoke
According to radiation treatment is carried out in instrument, taken out after 10 ~ 15min spare;
(2)Modification liquid is prepared:
Methyl hexadecanoate and glycerine are put into reaction kettle jointly, then add the potassium hydroxide of its gross mass 2 ~ 4%, constantly
After 8 ~ 12min of stir process, then acrylic polyoxyethylene ether is added into reaction kettle, while the temperature of reaction kettle is heated and is kept
For 80 ~ 85 DEG C, and the pressure in reaction kettle is risen into 0.4 ~ 0.5MPa, modification liquid is taken out to obtain after being stirred continuously 30 ~ 35min of processing
It is spare;
(3)Surface modification treatment:
By step(1)Nano-ceramic powder after processing is immersed in step(2)In obtained modification liquid, heating keeps the temperature of modification liquid
Spend for 65 ~ 70 DEG C, filtered after 1 ~ 1.5h of immersion treatment, it is spare to obtain filter residue;
(4)Drying process:
By step(3)The filter residue of gained, which is put into drying box, is dried processing, and it is 90 ~ 95 to keep the temperature in drying box
DEG C, taken out after handling 1 ~ 2h.
Further, step(1)Described in phosphoric acid solution mass fraction be 8 ~ 10%, while immersion treatment also
High-speed stirred processing is carried out, the rotating speed for controlling high-speed stirred is 2000 ~ 2400 revs/min.
Further, step(1)Described in the output power of ultraviolet irradiation instrument be 1800 ~ 2000W, ultraviolet
Wavelength is 270 ~ 290nm.
Further, step(2)Described in methyl hexadecanoate and glycerine mixing molar ratio be 2.2 ~ 2.7:1.
Further, step(2)Described in the addition of acrylic polyoxyethylene ether be methyl hexadecanoate gross mass
23~27%。
Further, step(3)Described in also carry out ultrasonic irradiation processing while immersion treatment, control ultrasound
The frequency of ripple is 140 ~ 150kHz.
Further, step(4)Described in drying process when the thickness that tiles in drying box of control filter residue be not more than
5cm。
The present invention has carried out nano-ceramic powder special surface modification treatment, wherein first carrying out acid soak to it, goes
Except the impurity on surface, pre-activate is realized, ultraviolet irradiation processing has then been carried out, using high energy ultraviolet to nano ceramics
Powder has carried out re-activation processing, improves the reaction active groups content and species on nano-ceramic powder surface, improves its work
Property, beneficial to follow-up modification, a kind of special modification liquid is then prepared, it is a kind of tripalmitin polyoxyethylene
Ether activator solution, can effectively change the surface hydrophilicity of nano-ceramic powder, enhance its lipophile, and improve its surface
Reactivity and dispersiveness, enhance its filling in coating and use quality.
The present invention has the following advantages compared with prior art:
The present invention has carried out special modification to the surface of nano-ceramic powder, and the surface for effectively improving nano-ceramic powder is lived
Property, its dispersing uniformity and respond in coating is improved, enhances the effect that its filling uses, and then improves painting
The quality of material, has good value for applications.
Embodiment
Embodiment 1
A kind of surface modifying method of nano-ceramic powder, includes the following steps:
(1)Surface activation process:
Nano-ceramic powder is put into phosphoric acid solution, is filtered out after immersion treatment 6min, then puts it into ultraviolet irradiation
Radiation treatment is carried out in instrument, is taken out after 10min spare;
(2)Modification liquid is prepared:
Methyl hexadecanoate and glycerine are put into reaction kettle jointly, the potassium hydroxide of its gross mass 2% is then added, constantly stirs
After mixing processing 8min, then acrylic polyoxyethylene ether is added into reaction kettle, while the temperature heating of reaction kettle is remained 80
DEG C, and the pressure in reaction kettle is risen into 0.4MPa, be stirred continuously after processing 30min take out modification liquid is spare;
(3)Surface modification treatment:
By step(1)Nano-ceramic powder after processing is immersed in step(2)In obtained modification liquid, heating keeps the temperature of modification liquid
Spend for 65 DEG C, filtered after immersion treatment 1h, it is spare to obtain filter residue;
(4)Drying process:
By step(3)The filter residue of gained, which is put into drying box, is dried processing, and it is 90 DEG C to keep the temperature in drying box, place
Taken out after managing 1h.
Further, step(1)Described in phosphoric acid solution mass fraction be 8%, also carried out while immersion treatment
High-speed stirred processing, the rotating speed for controlling high-speed stirred are 2000 revs/min.
Further, step(1)Described in the output power of ultraviolet irradiation instrument be 1800W, the wavelength of ultraviolet
For 270 ~ 275nm.
Further, step(2)Described in methyl hexadecanoate and glycerine mixing molar ratio be 2.2:1.
Further, step(2)Described in the addition of acrylic polyoxyethylene ether be methyl hexadecanoate gross mass
23%。
Further, step(3)Described in also carry out ultrasonic irradiation processing while immersion treatment, control ultrasound
The frequency of ripple is 140kHz.
Further, step(4)Described in drying process when the thickness that tiles in drying box of control filter residue be not more than
5cm。
Embodiment 2
A kind of surface modifying method of nano-ceramic powder, includes the following steps:
(1)Surface activation process:
Nano-ceramic powder is put into phosphoric acid solution, is filtered out after immersion treatment 7min, then puts it into ultraviolet irradiation
Radiation treatment is carried out in instrument, is taken out after 13min spare;
(2)Modification liquid is prepared:
Methyl hexadecanoate and glycerine are put into reaction kettle jointly, the potassium hydroxide of its gross mass 3% is then added, constantly stirs
After mixing processing 10min, then acrylic polyoxyethylene ether is added into reaction kettle, while the temperature heating of reaction kettle is remained 82
DEG C, and the pressure in reaction kettle is risen into 0.45MPa, be stirred continuously after processing 33min take out modification liquid is spare;
(3)Surface modification treatment:
By step(1)Nano-ceramic powder after processing is immersed in step(2)In obtained modification liquid, heating keeps the temperature of modification liquid
Spend for 67 DEG C, filtered after immersion treatment 1.2h, it is spare to obtain filter residue;
(4)Drying process:
By step(3)The filter residue of gained, which is put into drying box, is dried processing, and it is 92 DEG C to keep the temperature in drying box, place
Taken out after managing 1.6h.
Further, step(1)Described in phosphoric acid solution mass fraction be 9%, also carried out while immersion treatment
High-speed stirred processing, the rotating speed for controlling high-speed stirred are 2200 revs/min.
Further, step(1)Described in the output power of ultraviolet irradiation instrument be 1900W, the wavelength of ultraviolet
For 275 ~ 280nm.
Further, step(2)Described in methyl hexadecanoate and glycerine mixing molar ratio be 2.6:1.
Further, step(2)Described in the addition of acrylic polyoxyethylene ether be methyl hexadecanoate gross mass
25%。
Further, step(3)Described in also carry out ultrasonic irradiation processing while immersion treatment, control ultrasound
The frequency of ripple is 145kHz.
Further, step(4)Described in drying process when the thickness that tiles in drying box of control filter residue be not more than
5cm。
Embodiment 3
A kind of surface modifying method of nano-ceramic powder, includes the following steps:
(1)Surface activation process:
Nano-ceramic powder is put into phosphoric acid solution, is filtered out after immersion treatment 8min, then puts it into ultraviolet irradiation
Radiation treatment is carried out in instrument, is taken out after 15min spare;
(2)Modification liquid is prepared:
Methyl hexadecanoate and glycerine are put into reaction kettle jointly, the potassium hydroxide of its gross mass 4% is then added, constantly stirs
After mixing processing 12min, then acrylic polyoxyethylene ether is added into reaction kettle, while the temperature heating of reaction kettle is remained 85
DEG C, and the pressure in reaction kettle is risen into 0.5MPa, be stirred continuously after processing 35min take out modification liquid is spare;
(3)Surface modification treatment:
By step(1)Nano-ceramic powder after processing is immersed in step(2)In obtained modification liquid, heating keeps the temperature of modification liquid
Spend for 70 DEG C, filtered after immersion treatment 1.5h, it is spare to obtain filter residue;
(4)Drying process:
By step(3)The filter residue of gained, which is put into drying box, is dried processing, and it is 95 DEG C to keep the temperature in drying box, place
Taken out after managing 2h.
Further, step(1)Described in phosphoric acid solution mass fraction be 10%, while immersion treatment also into
The processing of row high-speed stirred, the rotating speed for controlling high-speed stirred are 2400 revs/min.
Further, step(1)Described in the output power of ultraviolet irradiation instrument be 2000W, the wavelength of ultraviolet
For 285 ~ 290nm.
Further, step(2)Described in methyl hexadecanoate and glycerine mixing molar ratio be 2.7:1.
Further, step(2)Described in the addition of acrylic polyoxyethylene ether be methyl hexadecanoate gross mass
27%。
Further, step(3)Described in also carry out ultrasonic irradiation processing while immersion treatment, control ultrasound
The frequency of ripple is 150kHz.
Further, step(4)Described in drying process when the thickness that tiles in drying box of control filter residue be not more than
5cm。
Comparative example 1
This comparative example 1 compared with Example 2, eliminates step(1)Surface activation process, method and step in addition are homogeneous
Together.
Comparative example 2
This comparative example 2 compared with Example 2, in step(3)With commercially available silane coupling agent kh550 in surface modification treatment
Substituting modification liquid component, method and step all same in addition.
Control group
Existing nano-ceramic powder surface modifying treatment, specifically first by ethanol, silane coupling agent kh550, water according to weight
Measure ratio 1:2:10 carry out being mixed to prepare treatment fluid, and then nano-ceramic powder is immersed in treatment fluid, ultrasonic under mechanical stirring
Filtered out after decentralized processing 20min, drying.
In order to contrast effect of the present invention, above-described embodiment 2, comparative example 1, comparative example 2, control group are corresponded into system
The nano-ceramic powder obtained is used in the making of coating, specifically corresponds to epoxy resin, nano-ceramic powder, curing agent, thixotropic agent
According to weight ratio 100:15:2:3, which carry out mixing, is put into agitator tank, to be taken after 800 revs/min of rotating speed stir process 1h
Go out, coating is made, finally the characteristic of coating is tested, specific correction data is as shown in table 1 below:
Table 1
Hardness after curing(H) | Wearability(Ten thousand times) | Thermal shock(It is secondary) | |
Embodiment 2 | 7H | 6.88 | 158 |
Comparative example 1 | 6H | 6.12 | 132 |
Comparative example 2 | 5H | 5.54 | 120 |
Control group | 5H | 5.32 | 110 |
Note:Wearability described in upper table 1 is to scrape wiper heavy burden 5.2kg with 3M to carry out frictional experiment;The thermal shock is
25 DEG C/350 DEG C cold cycling treatments are carried out, average minimum cycle-index when observation coating is without exception.
Nano-ceramic powder after the method for the present invention processing it can be seen from upper table 1, which has preferably to fill, uses quality, has
Effect enhances the performance of coating, great application value.
Claims (7)
1. a kind of surface modifying method of nano-ceramic powder, it is characterised in that include the following steps:
(1)Surface activation process:
Nano-ceramic powder is put into phosphoric acid solution, is filtered out after 6 ~ 8min of immersion treatment, then puts it into ultraviolet spoke
According to radiation treatment is carried out in instrument, taken out after 10 ~ 15min spare;
(2)Modification liquid is prepared:
Methyl hexadecanoate and glycerine are put into reaction kettle jointly, then add the potassium hydroxide of its gross mass 2 ~ 4%, constantly
After 8 ~ 12min of stir process, then acrylic polyoxyethylene ether is added into reaction kettle, while the temperature of reaction kettle is heated and is kept
For 80 ~ 85 DEG C, and the pressure in reaction kettle is risen into 0.4 ~ 0.5MPa, modification liquid is taken out to obtain after being stirred continuously 30 ~ 35min of processing
It is spare;
(3)Surface modification treatment:
By step(1)Nano-ceramic powder after processing is immersed in step(2)In obtained modification liquid, heating keeps the temperature of modification liquid
Spend for 65 ~ 70 DEG C, filtered after 1 ~ 1.5h of immersion treatment, it is spare to obtain filter residue;
(4)Drying process:
By step(3)The filter residue of gained, which is put into drying box, is dried processing, and it is 90 ~ 95 to keep the temperature in drying box
DEG C, taken out after handling 1 ~ 2h.
A kind of 2. surface modifying method of nano-ceramic powder according to claim 1, it is characterised in that step(1)Middle institute
The mass fraction for the phosphoric acid solution stated is 8 ~ 10%, and high-speed stirred processing is also carried out while immersion treatment, controls high-speed stirred
Rotating speed be 2000 ~ 2400 revs/min.
A kind of 3. surface modifying method of nano-ceramic powder according to claim 1, it is characterised in that step(1)Middle institute
The output power for the ultraviolet irradiation instrument stated is 1800 ~ 2000W, and the wavelength of ultraviolet is 270 ~ 290nm.
A kind of 4. surface modifying method of nano-ceramic powder according to claim 1, it is characterised in that step(2)Middle institute
The molar ratio for methyl hexadecanoate and the glycerine mixing stated is 2.2 ~ 2.7:1.
A kind of 5. surface modifying method of nano-ceramic powder according to claim 1, it is characterised in that step(2)Middle institute
The addition for the acrylic polyoxyethylene ether stated is the 23 ~ 27% of methyl hexadecanoate gross mass.
A kind of 6. surface modifying method of nano-ceramic powder according to claim 1, it is characterised in that step(3)Middle institute
That states also carries out ultrasonic irradiation processing while immersion treatment, and the frequency for controlling ultrasonic wave is 140 ~ 150kHz.
A kind of 7. surface modifying method of nano-ceramic powder according to claim 1, it is characterised in that step(4)Middle institute
The thickness for controlling filter residue to tile in drying box during the drying process stated is not more than 5cm.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN108752723A (en) * | 2018-05-28 | 2018-11-06 | 赵锋 | A kind of preparation method of thermal conductivity plastic composite |
CN108997783A (en) * | 2018-05-28 | 2018-12-14 | 赵锋 | A kind of processing method of the inorganic pigment for dyeing of plastics |
CN112853227A (en) * | 2021-01-09 | 2021-05-28 | 广州慧能新材料科技有限公司 | Corrosion-resistant powder metallurgy composite material and preparation method thereof |
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CN103304711A (en) * | 2013-06-19 | 2013-09-18 | 中南大学 | Preparation method of resin-wrapped aluminum hydroxide |
CN107311521A (en) * | 2017-07-12 | 2017-11-03 | 合肥雅克丽新型建材有限公司 | A kind of preparation method of novel anticorrosion insulation material |
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CN1473883A (en) * | 2003-07-01 | 2004-02-11 | 上海华明高技术(集团)有限公司 | Method for increasing dispersiveness of inorganic oxide powder in organic medium |
CN103304711A (en) * | 2013-06-19 | 2013-09-18 | 中南大学 | Preparation method of resin-wrapped aluminum hydroxide |
CN107311521A (en) * | 2017-07-12 | 2017-11-03 | 合肥雅克丽新型建材有限公司 | A kind of preparation method of novel anticorrosion insulation material |
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CN108752723A (en) * | 2018-05-28 | 2018-11-06 | 赵锋 | A kind of preparation method of thermal conductivity plastic composite |
CN108997783A (en) * | 2018-05-28 | 2018-12-14 | 赵锋 | A kind of processing method of the inorganic pigment for dyeing of plastics |
CN112853227A (en) * | 2021-01-09 | 2021-05-28 | 广州慧能新材料科技有限公司 | Corrosion-resistant powder metallurgy composite material and preparation method thereof |
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