CN109535773B - Preparation method of imidazoline-zinc oxide composite powder - Google Patents
Preparation method of imidazoline-zinc oxide composite powder Download PDFInfo
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- CN109535773B CN109535773B CN201811551186.4A CN201811551186A CN109535773B CN 109535773 B CN109535773 B CN 109535773B CN 201811551186 A CN201811551186 A CN 201811551186A CN 109535773 B CN109535773 B CN 109535773B
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- imidazoline
- zinc oxide
- composite powder
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- oxide composite
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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
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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
- 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
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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
- C09D5/08—Anti-corrosive paints
Abstract
The invention relates to a preparation technology of a metal coating anticorrosive material, and aims to provide a preparation method of imidazoline-zinc oxide composite powder. The method comprises the following steps: mixing zinc acetate dihydrate, diglycol and imidazoline under stirring, and heating to fully dissolve; heating to 140-160 ℃, condensing, refluxing, and stirring for reaction; after the reaction is finished, centrifugal separation is carried out, and the precipitate is washed by absolute ethyl alcohol and dried to prepare the imidazoline-zinc oxide composite powder. The preparation process is simple, and the silicon oxide-coated core-shell material can be directly prepared by taking zinc oxide as a core material. When the hollow silica microsphere is used subsequently, only hydrochloric acid is used for dissolving zinc oxide, imidazoline can be left in the silica shell, and the complex process of impregnating and loading imidazoline by the hollow silica microsphere is avoided. The loading capacity of imidazoline can be further improved, more imidazoline can be added after being coated without directly contacting with the coating, and the addition amount of the imidazoline can be increased.
Description
Technical Field
The invention relates to a preparation technology of a metal coating anticorrosive material, in particular to a preparation method of imidazoline-zinc oxide composite powder.
Background
Zinc oxide is used as a semiconductor amphoteric oxide, has a wide application range, and is often used as a core material in a preparation process of a core-shell material. Imidazoline is a corrosion inhibitor material and is widely applied to metal anticorrosive coatings.
In the prior art, hollow silica microspheres are usually used for impregnating and loading imidazoline, but the impregnation and loading process is complex, and corrosion inhibitor imidazoline cannot be added in the metal anticorrosive coating too much (the dosage is generally within three thousandth).
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects in the prior art and provides a preparation method of imidazoline-zinc oxide composite powder.
In order to solve the technical problem, the solution of the invention is as follows:
the preparation method of the imidazoline-zinc oxide composite powder comprises the following steps:
(1) under the condition of stirring, adding 0.02mol of zinc acetate dihydrate, 100ml of diglycol and 0.01-0.02 mol of imidazoline into a three-neck flask, heating in an oil bath to 100 ℃, and stirring for 1h to fully dissolve;
(2) heating the oil bath to 140-160 ℃, condensing and refluxing, and stirring for reaction for 4-6 h;
(3) taking out the three-neck flask from the oil bath, and placing the three-neck flask into cold water to terminate the reaction;
(4) separating the liquid in the three-mouth flask by using a centrifugal separator, and centrifugally washing the obtained precipitate twice by using absolute ethyl alcohol;
(5) and drying the precipitate in an oven to obtain the imidazoline-zinc oxide composite powder.
In the invention, the stirring speed in the step (1) is 200 r/min.
In the invention, the rotation speed of the centrifugal separator in the step (4) is 12000rpm, and the centrifugal separation time is 10 min.
In the invention, the rotation speed of the centrifugal washing in the step (4) is 12000rpm, and the washing time is 10 min.
In the invention, the drying temperature in the step (5) is 80 ℃.
In the invention, the imidazoline is a product of an Aladdin industry company, and the purity is 99%. The zinc acetate dihydrate is a product of the Aladdin industry company, and the purity is 99%.
Compared with the prior art, the invention has the following beneficial effects:
1. the preparation process is simple, and the silicon oxide-coated core-shell material can be directly prepared by taking zinc oxide as a core material. When the paint is used subsequently, only hydrochloric acid is used for dissolving zinc oxide, imidazoline can be left in the silica shell (used for being added in the metal anticorrosive paint), and the complex process of impregnating and loading imidazoline by the hollow silica microspheres is avoided.
2. The imidazoline-zinc oxide composite powder can further improve the loading capacity of imidazoline, and compared with the loading capacity of a hollow silica microsphere impregnation loading imidazoline technology which is less than 20%, the loading capacity of the imidazoline-zinc oxide composite powder can be improved to be more than 30%.
3. The coated imidazoline can be added more without directly contacting with the coating, so that the compact structure of the final coating is not influenced by the increase of the imidazoline. Under the coating, the addition amount of imidazoline can be increased to a few percent (10 times higher than the prior art).
Detailed Description
According to the invention, zinc oxide and imidazoline are compounded to prepare the imidazoline-zinc oxide composite powder, and the subsequent coating of the imidazoline-zinc oxide composite powder can simplify the loading process of the imidazoline hollow microsphere and expand the application range of imidazoline materials. In the invention, the reagents are all commercial products. For example, imidazoline is an alatin reagent, ltd, with a purity of 99%. Zinc acetate dihydrate is an Allantin reagent, Inc., with a purity of 99%.
The invention is further described below by way of examples.
Example 1
1. Under the stirring condition of 200r/min, adding 0.02mol of zinc acetate dihydrate and 100ml of diethylene glycol into a three-neck flask, simultaneously adding 0.01mol of imidazoline, heating the oil bath to 100 ℃, and stirring for 1h to fully dissolve the zinc acetate dihydrate and the diethylene glycol;
2. then heating the oil bath to 160 ℃, condensing and refluxing, and stirring for reaction for 4 hours;
3. taking out the flask from the oil bath, and placing the flask into cold water to terminate the reaction;
4. separating the liquid in the flask by a centrifugal separator (12000rpm, 10min), and centrifugally washing the obtained precipitate twice by absolute ethyl alcohol (12000rpm, 10 min);
5. and drying the precipitate in an oven at 80 ℃ to obtain the imidazoline-zinc oxide composite powder material.
Example 2
1. Under the stirring condition of 200r/min, adding 0.02mol of zinc acetate dihydrate and 100ml of diethylene glycol into a three-neck flask, simultaneously adding 0.015mol of imidazoline, heating the oil bath to 100 ℃, and stirring for 1h to fully dissolve the zinc acetate dihydrate and the diethylene glycol;
2. then heating the oil bath to 140 ℃, condensing and refluxing, and stirring for reaction for 6 hours;
3. taking out the flask from the oil bath, and placing the flask into cold water to terminate the reaction;
4. separating the liquid in the flask by a centrifugal separator (12000rpm, 10min), and centrifugally washing the obtained precipitate twice by absolute ethyl alcohol (12000rpm, 10 min);
5. and drying the precipitate in an oven at 80 ℃ to obtain the imidazoline-zinc oxide composite powder material.
Example 3
1. Under the stirring condition of 200r/min, adding 0.02mol of zinc acetate dihydrate and 100ml of diethylene glycol into a three-neck flask, simultaneously adding 0.02mol of imidazoline, heating the oil bath to 100 ℃, and stirring for 1h to fully dissolve the zinc acetate dihydrate and the diethylene glycol;
2. then heating the oil bath to 150 ℃, condensing and refluxing, and stirring for reaction for 5 hours;
3. taking out the flask from the oil bath, and placing the flask into cold water to terminate the reaction;
4. separating the liquid in the flask by a centrifugal separator (12000rpm, 10min), and centrifugally washing the obtained precipitate twice by absolute ethyl alcohol (12000rpm, 10 min);
5. and drying the precipitate in an oven at 80 ℃ to obtain the imidazoline-zinc oxide composite powder material.
Application example:
1. the imidazoline-zinc oxide composite powder prepared by the invention has the specific application method that:
dispersing 0.5g of imidazoline-zinc oxide composite powder into 20ml of ethanol, adding 9g of deionized water and 1ml of 25% ammonia water by mass fraction, and uniformly mixing; adding 0.5ml of tetraethoxysilane into the mixture to react for 1 hour, and centrifugally separating formed precipitates by using a centrifugal machine; adding the precipitate into 50ml of 5% hydrochloric acid aqueous solution by mass, soaking for 8 hours, and then performing centrifugal precipitation twice by using deionized water; drying at 80 ℃ to obtain the imidazoline loaded silicon dioxide microspheres.
2. The addition method of the coated product in the metal anticorrosive paint comprises the following steps:
weighing imidazoline-loaded silica microspheres according to 3-5% of the mass of the coating, adding the imidazoline-loaded silica microspheres into the coating in batches before coating spraying, dispersing for 1 hour by using a dispersion machine, and rotating at 1000rpm to obtain the coating added with the corrosion inhibitor-loaded silica microspheres.
Claims (4)
1. The preparation method of the imidazoline-zinc oxide composite powder is characterized by comprising the following steps:
(1) under the condition of stirring, adding 0.02mol of zinc acetate dihydrate, 100ml of diglycol and 0.01-0.02 mol of imidazoline into a three-neck flask, heating in an oil bath to 100 ℃, and stirring for 1h to fully dissolve;
(2) heating the oil bath to 140-160 ℃, and reacting for 4-6 hours under the conditions of condensation reflux and stirring;
(3) taking out the three-neck flask from the oil bath, and placing the three-neck flask into cold water to terminate the reaction;
(4) separating the liquid in the three-mouth flask by using a centrifugal separator, and centrifugally washing the obtained precipitate twice by using absolute ethyl alcohol; the rotating speed of the centrifugal separator is 12000rpm, and the centrifugal separation time is 10 min; the rotating speed during centrifugal washing is 12000rpm, and the washing time is 10 min;
(5) and drying the precipitate in an oven to obtain the imidazoline-zinc oxide composite powder.
2. The method according to claim 1, wherein the stirring rate in the step (1) is 200 r/min.
3. The method as claimed in claim 1, wherein the drying temperature in the step (5) is 80 ℃.
4. The method of claim 1, wherein the imidazoline is a product of the alatin industries, 99% pure; the zinc acetate dihydrate is a product of the Aladdin industry company, and the purity is 99%.
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| Application Number | Priority Date | Filing Date | Title |
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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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| CN201811551186.4A CN109535773B (en) | 2018-12-18 | 2018-12-18 | Preparation method of imidazoline-zinc oxide composite powder |
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| CN109535773A CN109535773A (en) | 2019-03-29 |
| CN109535773B true CN109535773B (en) | 2020-12-11 |
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| 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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| 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 |
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2018
- 2018-12-18 CN CN201811551186.4A patent/CN109535773B/en active Active
Patent Citations (4)
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| 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 |
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