CN109535773A - A kind of preparation method of imidazoline-zinc oxide composite powder - Google Patents
A kind of preparation method of imidazoline-zinc oxide composite powder Download PDFInfo
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- CN109535773A CN109535773A CN201811551186.4A CN201811551186A CN109535773A CN 109535773 A CN109535773 A CN 109535773A CN 201811551186 A CN201811551186 A CN 201811551186A CN 109535773 A CN109535773 A CN 109535773A
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- Prior art keywords
- imidazoline
- zinc oxide
- composite powder
- oxide composite
- oil bath
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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
- C09C1/04—Compounds of zinc
- C09C1/043—Zinc oxide
-
- 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
- C09C3/063—Coating
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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
-
- 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
- C09D5/08—Anti-corrosive paints
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Paints Or Removers (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
The present invention relates to metal coating anti-corrosion material technologies of preparing, it is desirable to provide a kind of preparation method of imidazoline-zinc oxide composite powder.It include: under stiring to mix zinc acetate dihydrate, diethylene glycol (DEG) and imidazoline, heating makes sufficiently to dissolve；140~160 DEG C of condensing refluxes are warming up to, are stirred to react；Centrifuge separation is used after terminating reaction, precipitating is washed with dehydrated alcohol, dried, and imidazoline-zinc oxide composite powder is made.Preparation process of the present invention is simple, can directly prepare the core-shell material of cladding silica as nuclear material by zinc oxide.As long as subsequent in use, can be stayed in imidazoline in silica shell using dissolving with hydrochloric acid zinc oxide, avoid the complicated technology of controlled hollow silicon oxide microsphere dip loading imidazoline.The load capacity that can be further improved imidazoline, the imidazoline after cladding can add more without direct and coating contacts, and the additive amount of imidazoline can be improved.
Description
Technical field
The present invention relates to metal coating anti-corrosion material technology of preparing, in particular to a kind of imidazoline-zinc oxide composite powder
Preparation method.
Background technique
Zinc oxide is of wide application as a kind of semiconductor amphoteric oxide, especially in the preparation process of core-shell material
In be often taken as inner nuclear material application.Imidazoline is a kind of inhibition agent material, is widely used in metal anti-corrosive paint.
In the prior art usually using controlled hollow silicon oxide microsphere dip loading imidazoline, but the technical process ratio of dip loading
It is more complex, and corrosion inhibiter imidazoline cannot add (general dosage is within 3/1000ths) too much in metal anti-corrosive paint.
Summary of the invention
The technical problem to be solved by the present invention is to overcome deficiency in the prior art, it is multiple to provide a kind of imidazoline-zinc oxide
Close raw powder's production technology.
In order to solve the technical problem, solution of the invention is:
A kind of preparation method of imidazoline-zinc oxide composite powder is provided, is included the following steps:
(1) under agitation, be added into three-necked flask 0.02mol zinc acetate dihydrate, 100ml diethylene glycol (DEG) and 0.01~
The imidazoline of 0.02mol, oil bath are warming up to 100 DEG C of stirring 1h, make sufficiently to dissolve；
(2) oil bath is warming up to 140~160 DEG C, is condensed back, is stirred to react 4~6h；
(3) three-necked flask is taken out from oil bath, is placed in cold water and is terminated reaction；
(4) liquid in three-necked flask is separated with centrifugal separator, obtained precipitating dehydrated alcohol centrifuge washing two
It is secondary；
(5) sediment is dried in an oven, obtains imidazoline-zinc oxide composite powder.
In the present invention, the stirring rate in the step (1) is 200r/min.
In the present invention, the revolving speed of centrifugal separator is 12000rpm in the step (4), and the centrifuge separation time is 10min.
In the present invention, the revolving speed in the step (4) when centrifuge washing is 12000rpm, wash time 10min.
In the present invention, the drying temperature in the step (5) is 80 DEG C.
In the present invention, the imidazoline is Aladdin industrial group product, purity 99%.The zinc acetate dihydrate be Ah
Latin industrial group product, purity 99%.
Compared with existing technology of preparing, the invention has the following advantages:
1, preparation process of the present invention is simple, can directly prepare the nucleocapsid material of cladding silica as nuclear material by zinc oxide
Material.As long as subsequent in use, can be stayed in imidazoline in silica shell using dissolving with hydrochloric acid zinc oxide (in metal
Addition in anticorrosive paint), avoid the complicated technology of controlled hollow silicon oxide microsphere dip loading imidazoline.
2, it can be further improved the load capacity of imidazoline using imidazoline-zinc oxide composite powder of the invention, relatively
In load capacity of the controlled hollow silicon oxide microsphere dip loading imidazoline technology less than 20%, using imidazoline-zinc oxide of the invention
Load capacity can be increased to 30% or more by composite granule.
3, the imidazoline after cladding can add more without direct and coating contacts, in this way will not be because of imidazoline
Increase and influence the compact texture of final coating.Under this cladding, a few percent is can be improved in the additive amount of imidazoline
(10 times can be improved compared with the existing technology).
Specific embodiment
The present invention by zinc oxide and imidazoline carry out it is compound prepare imidazoline-zinc oxide composite powder, by subsequent to miaow
Oxazoline-zinc oxide composite powder cladding can simplify the load process of imidazoline hollow microsphere, expand the application of imidazoline material
Range.In the present invention, the reagent is commercial products.For example, imidazoline is Aladdin reagent Co., Ltd, purity 99%.
Zinc acetate dihydrate is Aladdin reagent Co., Ltd, purity 99%.
The present invention will be further described below by way of example.
Embodiment 1
1. 0.02mol zinc acetate dihydrate is added into three-necked flask and 100ml bis- is sweet under the stirring condition of 200r/min
Alcohol, while the imidazoline of 0.01mol is added, oil bath is warming up to 100 DEG C of stirring 1h and is allowed to sufficiently dissolve；
2. oil bath is warming up to 160 DEG C after, is condensed back, is stirred to react 4h；
3. taking out flask from oil bath, it is placed in cold water and terminates reaction；
4. the centrifugal separator of the liquid in flask is separated (12000rpm, 10min), obtained precipitating dehydrated alcohol
Centrifuge washing (12000rpm, 10min) is twice；
5. sediment is dried in 80 DEG C of baking ovens and obtains imidazoline-zinc oxide composite powder material.
Embodiment 2
1. 0.02mol zinc acetate dihydrate is added into three-necked flask and 100ml bis- is sweet under the stirring condition of 200r/min
Alcohol, while the imidazoline of 0.015mol is added, oil bath is warming up to 100 DEG C of stirring 1h and is allowed to sufficiently dissolve；
2. oil bath is warming up to 140 DEG C after, is condensed back, is stirred to react 6h；
3. taking out flask from oil bath, it is placed in cold water and terminates reaction；
4. the centrifugal separator of the liquid in flask is separated (12000rpm, 10min), obtained precipitating dehydrated alcohol
Centrifuge washing (12000rpm, 10min) is twice；
5. sediment is dried in 80 DEG C of baking ovens and obtains imidazoline-zinc oxide composite powder material.
Embodiment 3
1. 0.02mol zinc acetate dihydrate is added into three-necked flask and 100ml bis- is sweet under the stirring condition of 200r/min
Alcohol, while the imidazoline of 0.02mol is added, oil bath is warming up to 100 DEG C of stirring 1h and is allowed to sufficiently dissolve；
2. oil bath is warming up to 150 DEG C after, is condensed back, is stirred to react 5h；
3. taking out flask from oil bath, it is placed in cold water and terminates reaction；
4. the centrifugal separator of the liquid in flask is separated (12000rpm, 10min), obtained precipitating dehydrated alcohol
Centrifuge washing (12000rpm, 10min) is twice；
5. sediment is dried in 80 DEG C of baking ovens and obtains imidazoline-zinc oxide composite powder material.
Using example:
1, imidazoline-zinc oxide composite powder that the present invention prepares, concrete application method:
It takes 0.5g imidazoline-zinc oxide composite powder to be scattered in 20ml ethyl alcohol, 9g deionized water and 1ml mass point is added
The ammonium hydroxide that number is 25% is uniformly mixed；Take 0.5ml ethyl orthosilicate to be added in mixture to react 1 hour, the precipitating of formation with from
Scheming centrifuge separation；Precipitating is added in the aqueous hydrochloric acid solution that 50ml mass fraction is 5% and is impregnated 8 hours, deionization is then used
Water centrifugation is twice；It is dried at 80 DEG C, obtains the silicon dioxide microsphere of load imidazoline.
2, it is coated adding method of the product of processing in metal anti-corrosive paint:
Painting is added portionwise before coating spraying in the silicon dioxide microsphere for weighing load imidazoline by the 3~5% of coating quality
In material, dispersed 1 hour with dispersion machine, the coating of corrosion inhibiter nonloaded silica microballoon is added to get arriving by revolving speed 1000rpm.
Claims (6)
1. a kind of preparation method of imidazoline-zinc oxide composite powder, which comprises the steps of:
(1) under agitation, be added into three-necked flask 0.02mol zinc acetate dihydrate, 100ml diethylene glycol (DEG) and 0.01~
The imidazoline of 0.02mol, oil bath, which is warming up to 100 DEG C of stirring 1h, to be made sufficiently to dissolve；
(2) oil bath is warming up to 140~160 DEG C, is condensed back and stirs 4~6h of lower reaction；
(3) three-necked flask is taken out from oil bath, is placed in cold water and is terminated reaction；
(4) liquid in three-necked flask is separated with centrifugal separator, obtained precipitating with dehydrated alcohol centrifuge washing twice；
(5) sediment is dried in an oven, imidazoline-zinc oxide composite powder is made.
2. the method according to claim 1, wherein the stirring rate in the step (1) is 200r/min.
3. the method according to claim 1, wherein the revolving speed of centrifugal separator is in the step (4)
12000rpm, centrifuge separation time are 10min.
4. the method according to claim 1, wherein the revolving speed in the step (4) when centrifuge washing is
12000rpm, wash time 10min.
5. the method according to claim 1, wherein the drying temperature in the step (5) is 80 DEG C.
6. the method according to claim 1, wherein the imidazoline is Aladdin industrial group product, purity
It is 99%；The zinc acetate dihydrate is Aladdin industrial group product, purity 99%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811551186.4A CN109535773B (en) | 2018-12-18 | 2018-12-18 | Preparation method of imidazoline-zinc oxide composite powder |
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|---|---|---|---|
| CN201811551186.4A CN109535773B (en) | 2018-12-18 | 2018-12-18 | Preparation method of imidazoline-zinc oxide composite powder |
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| CN109535773A true CN109535773A (en) | 2019-03-29 |
| CN109535773B CN109535773B (en) | 2020-12-11 |
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| CN201811551186.4A Active CN109535773B (en) | 2018-12-18 | 2018-12-18 | Preparation method of imidazoline-zinc oxide composite powder |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113462199A (en) * | 2021-05-17 | 2021-10-01 | 北京化工大学 | Preparation method of inorganic oxide pigment filler loaded with composite corrosion inhibitor |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105062175A (en) * | 2015-08-10 | 2015-11-18 | 广西经正科技开发有限责任公司 | Antifouling biological adhesive agent and antifouling biological adhesive coating |
| CN108165085A (en) * | 2018-01-26 | 2018-06-15 | 成都新柯力化工科技有限公司 | A kind of preparation method of environment-friendly antibacterial water-based ink |
| CN108529662A (en) * | 2018-05-25 | 2018-09-14 | 洛阳理工学院 | A kind of method of modifying of nanometer Zinc oxide powder material |
| CN108795129A (en) * | 2018-06-25 | 2018-11-13 | 陕西科技大学 | A kind of preparation method of polyacrylate/benzotriazole@zinc oxide microcapsules composite anti-corrosive coatings |
-
2018
- 2018-12-18 CN CN201811551186.4A patent/CN109535773B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105062175A (en) * | 2015-08-10 | 2015-11-18 | 广西经正科技开发有限责任公司 | Antifouling biological adhesive agent and antifouling biological adhesive coating |
| CN108165085A (en) * | 2018-01-26 | 2018-06-15 | 成都新柯力化工科技有限公司 | A kind of preparation method of environment-friendly antibacterial water-based ink |
| CN108529662A (en) * | 2018-05-25 | 2018-09-14 | 洛阳理工学院 | A kind of method of modifying of nanometer Zinc oxide powder material |
| CN108795129A (en) * | 2018-06-25 | 2018-11-13 | 陕西科技大学 | A kind of preparation method of polyacrylate/benzotriazole@zinc oxide microcapsules composite anti-corrosive coatings |
Non-Patent Citations (3)
| Title |
|---|
| S.H. SONAWANE等: "Improved active anticorrosion using layer-by-layer assembled ZnO nanocontainers with benzotriazole", 《CHEMICAL ENGINEERING JOURNAL》 * |
| 孙传尧主编: "《选矿工程师手册》", 30 March 2015, 冶金工业出版社 * |
| 武婷婷等: "负载缓蚀剂的微米容器对涂层防腐性能的影响", 《电镀与涂饰》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113462199A (en) * | 2021-05-17 | 2021-10-01 | 北京化工大学 | Preparation method of inorganic oxide pigment filler loaded with composite corrosion inhibitor |
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