CN108504165A - A kind of preparation method of electrophoretic paint calcined kaolin clay filler - Google Patents
A kind of preparation method of electrophoretic paint calcined kaolin clay filler Download PDFInfo
- Publication number
- CN108504165A CN108504165A CN201810314771.6A CN201810314771A CN108504165A CN 108504165 A CN108504165 A CN 108504165A CN 201810314771 A CN201810314771 A CN 201810314771A CN 108504165 A CN108504165 A CN 108504165A
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- CN
- China
- Prior art keywords
- kaolin
- preparation
- electrophoretic paint
- clay filler
- kaolinic
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other 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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/44—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for electrophoretic applications
- C09D5/448—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for electrophoretic applications characterised by the additives used
Abstract
The invention discloses a kind of preparation method of electrophoretic paint calcined kaolin clay filler, for raw ore kaolin through a calcination processing, the crystallization water and foreign ion being stripped of in kaolin reduce its influence to electrodeposited paint film salt fog resistance in the present invention；It is handled again through sodium hydroxide alkali cleaning later, kaolin surface is set to form more microcellular structure, increase kaolinic porosity, again after ultramicro grinding, reach the granularity and decentralized standard of required kaolin product in electrophoretic painting, its absorption property, specific surface area improves, but simultaneously increase kaolinic oil absorbency, therefore using dissolving gel method, the aged formation hydrated titanium dioxide particle of TiO 2 sol system is coated on kaolin particle, it is handled again through secondary clacining, adhere to one layer of densification on kaoline par-tides surface, uniform spherical tio2 particle, significantly reduce kaolinic oil absorption, reduce influence of the kaolin oil absorption to electrophoretic coating and its film performance.
Description
Technical field
The invention belongs to the preparing technical fields of inorganic filler, and in particular to a kind of electrophoretic paint calcined kaolin clay filler
Preparation method.
Background technology
In the 60's of 20th century, as the epoch improve, the continuous improvement that people require Metal surface anti-corrosion antirust,
The generation of excessive metal corruption rust phenomenon in order to prevent, is alleviated with kaolinic property.It is commonly used in electrophoretic paint industry
Kaolin has two major classes：1) ultrafine kaolin is washed；2) calcined ultrafine kaolin.Calcined kaolin is developed recently
A kind of new function type filler, the filler as coating not only have higher whiteness and opacity, can be in high polymer
The characteristics such as preferable stability and color and luster are provided, and has preferable covering power, soft and wear-resisting, and has anti scuffing, do not shrink, holds
Easily realize the mechanization and automation of application industry, it is suitable complex-shaped, there are edge corner angle, a hole Workpiece coating, and other tables
Surface treatment technology cannot solve under the pressure of this demand, so electrophoretic paint is gradually developed, and in many economy
Field plays irreplaceable role, such as auto industry, hardware, aluminium section bar, engineering machinery, imitative gold ornaments.
In conjunction with domestic and international present Research, for calcined kaolin in the effect to electrophoretic paint, what is relied primarily on is current non-gold
Belong to one of most important deep process technology of mine：Its surface is modified.The modification of calcined kaolin surface refers to the needs according to application, is used
Physics, chemical or mechanical method is handled kaolin powder surface to change the physicochemical property on its surface, and height is made
Ridge soil subparticle surface coats one layer of organic coupling agent compound, to make kaolin surface property change, purpose
It is to enhance its compatibility between organic matter when using electrophoretic paint.
Invention content
The present invention provides a kind of preparation methods of electrophoretic paint calcined kaolin clay filler, significantly improve the anti-of electrodeposited paint film
Shrinkage cavity performance.
The present invention uses following technical scheme：
A kind of preparation method of electrophoretic paint calcined kaolin clay filler, includes the following steps：
（1）Primary calcining：
20-40g raw ore kaolin is placed in Muffle furnace and is being warming up to 630-680 DEG C of calcining 30-50min, is warming up to later
850-1050 DEG C of temperature lower calcination 1-2h, and furnace cooling take out for use；
（2）Alkali modification processing：
Kaolin after above-mentioned calcining and NaOH solution are stirred to react 18-24h under 85-93 DEG C of water bath with thermostatic control, wait for reaction eventually
Mixed solution is centrifuged when only, is washed, dry 10-14h, obtains alkaline-modified kaolin at 105-115 DEG C；
（3）Pulverization process：
Above-mentioned alkaline-modified kaolin is crushed using jaw crusher, its granularity is less than 20mm after being crushed, then through Raymond mill
Powder machine carries out ultra-fine grinding, and analyzer rotating speed is 1000r/min, and kaolin fineness adds kaolin after crushing in 300-350 mesh
Enter in appropriate deionization, carries out mechanical strong stirring, prepare kaolin ore slurry；
（4）Dissolving-gel method prepares titania modified kaolin：
After 3-6min is mixed in the butyl titanate of 5-7ml and appropriate absolute ethyl alcohol, 1mol/L hydrochloric acid solutions are added dropwise, adjust
Reaction system pH to 3.2-4.5 is prepared titanium salt presoma, then slowly drips precursor solution after stirring 50-70min
Being added in above-mentioned kaolin ore slurry makes its hydrolysis, and heating water bath is to 40-55 DEG C, insulated and stirred 3-4h, after being aged 12-20h later,
Again through being dehydrated, drying；
（5）Secondary clacining：
Kaolin-composite titania material after above-mentioned drying is placed in Muffle furnace in 680-950 DEG C of temperature lower calcination 2-
3h obtains coated by titanium dioxide kaolin composite material.
Wherein, the step（2）The concentration of middle NaOH solution is in 2-5mol/L, and sodium hydroxide and kaolinic ratio are in 5-
7mL/g。
Wherein, step（3）The concentration of middle kaolin ore slurry is in 11-15%.
Wherein, the step（4）Middle drying condition is 95-110 DEG C dry to constant weight, titanium dioxide and kaolinic quality
Than being 1:2-5.
Compared with prior art, beneficial benefit of the invention is as follows：
Raw ore kaolin is through a calcination processing in the present invention, be stripped of after being calcined at 650 DEG C or so kaolin surface part or
Whole hydroxyls, while it being stripped of water of constitution existing for kaolin internal crystallization water and OH- form, so that kaolin is had higher
Activity, then through high-temperature calcination, the carbon impurity in kaolin raw ore is eliminated, silica relative amount increases in kaolin, warp
The influence of the crystallization water and foreign ion to electrodeposited paint film salt fog resistance can almost be ignored not in kaolin after calcination processing
Meter；It is handled again through sodium hydroxide alkali cleaning later, a large amount of SiO in kaolin2Dissolution, makes its surface form more microcellular structure,
Kaolinic porosity is increased, then after ultramicro grinding, kaolin clay filler fine size, and dispersion performance is preferable, reaches electrophoresis
The granularity and decentralized standard of required kaolin product in application, absorption property, specific surface area improve, but make simultaneously kaolinic
Oil absorbency increases, therefore uses dissolving-gel method, by the aged formation hydrated titanium dioxide particle packet of TiO 2 sol system
It overlays on kaolin particle, then is handled through secondary clacining, adhere to one layer of fine and close, uniform spherical dioxy on kaoline par-tides surface
Change titanium particle, due to the coating function of TiO 2 particles, significantly reduces kaolinic oil absorption, reduce kaolin oil absorption
Influence to electrophoretic coating and its film performance.
Specific implementation mode
Embodiment 1
A kind of preparation method of electrophoretic paint calcined kaolin clay filler, includes the following steps：
（1）Primary calcining：
20g raw ore kaolin is placed in Muffle furnace and is being warming up to 650 DEG C of calcining 40min, is forged at a temperature of being warming up to 950 DEG C later
2h, and furnace cooling are burnt, is taken out for use；
（2）Alkali modification processing：
Kaolin after above-mentioned calcining and NaOH solution are stirred to react 18h under 90 DEG C of water bath with thermostatic control, it will when reaction terminating
Mixed solution is centrifuged, washs, and dry 12h, obtains alkaline-modified kaolin at 105 DEG C；
（3）Pulverization process：
Above-mentioned alkaline-modified kaolin is crushed using jaw crusher, its granularity is less than 20mm after being crushed, then through Raymond mill
Powder machine carries out ultra-fine grinding, and analyzer rotating speed is 1000r/min, and kaolin fineness adds kaolin after crushing in 300-350 mesh
Enter in appropriate deionization, carries out mechanical strong stirring, prepare kaolin ore slurry；
（4）Dissolving-gel method prepares titania modified kaolin：
After 5min is mixed in the butyl titanate of 6ml and appropriate absolute ethyl alcohol, 1mol/L hydrochloric acid solutions are added dropwise, adjust reaction
System pH to 3.5 is prepared titanium salt presoma, precursor solution is then slowly dropped to above-mentioned kaolinite after stirring 60min
Make its hydrolysis in native ore pulp, heating water bath is to 50 DEG C, insulated and stirred 3h, and after being aged 18h later, then through dehydration, 105 DEG C of dryings are extremely
Constant weight；
（5）Secondary clacining：
Kaolin-composite titania material after above-mentioned drying is placed in Muffle furnace in 750 DEG C of temperature lower calcination 3h, is obtained
Coated by titanium dioxide kaolin composite material.
Wherein, the step（2）The concentration of middle NaOH solution is in 4mol/L, and sodium hydroxide and kaolinic ratio are in 6mL/
g。
Wherein, step（3）The concentration of middle kaolin ore slurry is 13%.
Embodiment 2
A kind of preparation method of electrophoretic paint calcined kaolin clay filler, includes the following steps：
（1）Primary calcining：
20g raw ore kaolin is placed in Muffle furnace and is being warming up to 680 DEG C of calcining 30min, is warming up to later at a temperature of 1000 DEG C
2h, and furnace cooling are calcined, is taken out for use；
（2）Alkali modification processing：
Kaolin after above-mentioned calcining and NaOH solution are stirred to react 16h under 90 DEG C of water bath with thermostatic control, it will when reaction terminating
Mixed solution is centrifuged, washs, and dry 12h, obtains alkaline-modified kaolin at 105 DEG C；
（3）Pulverization process：
Above-mentioned alkaline-modified kaolin is crushed using jaw crusher, its granularity is less than 20mm after being crushed, then through Raymond mill
Powder machine carries out ultra-fine grinding, and analyzer rotating speed is 1000r/min, and kaolin fineness adds kaolin after crushing in 300-350 mesh
Enter in appropriate deionization, carries out mechanical strong stirring, prepare kaolin ore slurry；
（4）Dissolving-gel method prepares titania modified kaolin：
After 5min is mixed in the butyl titanate of 7ml and appropriate absolute ethyl alcohol, 1mol/L hydrochloric acid solutions are added dropwise, adjust reaction
System pH to 4.0 is prepared titanium salt presoma, precursor solution is then slowly dropped to above-mentioned kaolinite after stirring 60min
Make its hydrolysis in native ore pulp, heating water bath is to 50 DEG C, insulated and stirred 3h, and after being aged 18h later, then through dehydration, 105 DEG C of dryings are extremely
Constant weight；
（5）Secondary clacining：
Kaolin-composite titania material after above-mentioned drying is placed in Muffle furnace in 750 DEG C of temperature lower calcination 3h, is obtained
Coated by titanium dioxide kaolin composite material.
Wherein, the step（2）The concentration of middle NaOH solution is in 4mol/L, and sodium hydroxide and kaolinic ratio are in 6mL/
g。
Wherein, step（3）The concentration of middle kaolin ore slurry is 13%.
Claims (4)
1. a kind of preparation method of electrophoretic paint calcined kaolin clay filler, which is characterized in that include the following steps：
（1）Primary calcining：
20-40g raw ore kaolin is placed in Muffle furnace and is being warming up to 630-680 DEG C of calcining 30-50min, is warming up to later
850-1050 DEG C of temperature lower calcination 1-2h, and furnace cooling take out for use；
（2）Alkali modification processing：
Kaolin after above-mentioned calcining and NaOH solution are stirred to react 18-24h under 85-93 DEG C of water bath with thermostatic control, wait for reaction eventually
Mixed solution is centrifuged when only, is washed, dry 10-14h, obtains alkaline-modified kaolin at 105-115 DEG C；
（3）Pulverization process：
Above-mentioned alkaline-modified kaolin is crushed using jaw crusher, its granularity is less than 20mm after being crushed, then through Raymond mill
Powder machine carries out ultra-fine grinding, and analyzer rotating speed is 1000r/min, and kaolin fineness adds kaolin after crushing in 300-350 mesh
Enter in appropriate deionization, carries out mechanical strong stirring, prepare kaolin ore slurry；
（4）Dissolving-gel method prepares titania modified kaolin：
After 3-6min is mixed in the butyl titanate of 5-7ml and appropriate absolute ethyl alcohol, 1mol/L hydrochloric acid solutions are added dropwise, adjust
Reaction system pH to 3.2-4.5 is prepared titanium salt presoma, then slowly drips precursor solution after stirring 50-70min
Being added in above-mentioned kaolin ore slurry makes its hydrolysis, and heating water bath is to 40-55 DEG C, insulated and stirred 3-4h, after being aged 12-20h later,
Again through being dehydrated, drying；
（5）Secondary clacining：
Kaolin-composite titania material after above-mentioned drying is placed in Muffle furnace in 680-950 DEG C of temperature lower calcination 2-
3h obtains coated by titanium dioxide kaolin composite material.
2. a kind of preparation method of electrophoretic paint calcined kaolin clay filler according to claim 1, which is characterized in that described
Step（2）The concentration of middle NaOH solution is in 2-5mol/L, and sodium hydroxide and kaolinic ratio are in 5-7mL/g.
3. a kind of preparation method of electrophoretic paint calcined kaolin clay filler according to claim 1, which is characterized in that step
（3）The concentration of middle kaolin ore slurry is in 11-15%.
4. a kind of preparation method of electrophoretic paint calcined kaolin clay filler according to claim 1, which is characterized in that described
Step（4）Middle drying condition is 95-110 DEG C dry to constant weight, and titanium dioxide is 1 with kaolinic mass ratio:2-5.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810314771.6A CN108504165A (en) | 2018-04-10 | 2018-04-10 | A kind of preparation method of electrophoretic paint calcined kaolin clay filler |
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| CN201810314771.6A CN108504165A (en) | 2018-04-10 | 2018-04-10 | A kind of preparation method of electrophoretic paint calcined kaolin clay filler |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112375356A (en) * | 2020-11-27 | 2021-02-19 | 东莞全球环保科技有限公司 | Biodegradable soft shell forming process and mobile phone soft shell prepared by same |
| CN115926710A (en) * | 2022-11-25 | 2023-04-07 | 广州市高士实业有限公司 | Preparation of brightening glue |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1811058A (en) * | 2006-02-17 | 2006-08-02 | 上海东升新材料有限公司 | Composite titania material and its prepn and application |
-
2018
- 2018-04-10 CN CN201810314771.6A patent/CN108504165A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1811058A (en) * | 2006-02-17 | 2006-08-02 | 上海东升新材料有限公司 | Composite titania material and its prepn and application |
Non-Patent Citations (5)
| Title |
|---|
| 朱毅等: "《家具表面涂饰》", 31 August 2016, 东北林业大学出版社 * |
| 李金发等: "《鄂西煤系高岭土在药用橡胶中的应用研究》", 28 February 2013, 中国地质大学出版社有限责任公司 * |
| 毛建平: "白色颜填料的吸油量对粉末涂料性能的影响", 《涂料工业》 * |
| 王玉飞: "碱改性高岭土的吸油性能研究", 《榆林学院学报》 * |
| 陈洁渝等: "煅烧高岭土表面包覆二氧化钛实验研究", 《非金属矿》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112375356A (en) * | 2020-11-27 | 2021-02-19 | 东莞全球环保科技有限公司 | Biodegradable soft shell forming process and mobile phone soft shell prepared by same |
| CN115926710A (en) * | 2022-11-25 | 2023-04-07 | 广州市高士实业有限公司 | Preparation of brightening glue |
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Application publication date: 20180907 |