CN105086556A - Preparation method of nanometer particles used for anti-corrosion coating - Google Patents
Preparation method of nanometer particles used for anti-corrosion coating Download PDFInfo
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- CN105086556A CN105086556A CN201510490486.6A CN201510490486A CN105086556A CN 105086556 A CN105086556 A CN 105086556A CN 201510490486 A CN201510490486 A CN 201510490486A CN 105086556 A CN105086556 A CN 105086556A
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Abstract
The invention discloses a preparation method of nanometer particles used for an anti-corrosion coating. The grain size of the nanometer particles is controlled by regulating the pH value of a mother liquor system, and therefore multi-stage compound of the nanometer particles in the coating preparation process is achieved, and the compactness and the anti-corrosion performance of the nanometer coating are improved. Meanwhile, a modifying agent, namely, a silane coupling agent, is added in the preparation process of the nanometer particles, hydrophobization modification is conducted on the surfaces of the generated particles, and therefore the dispersity of the particles in the coating is improved, and the physicochemical property of the surfaces of the particles is improved. When the nanometer particles are placed in the coating instead of part of traditional non-nanometer-particle filler, cost can be reduced, the compactness and the anti-corrosion performance of the coating can be effectively improved, and the abrasion resistance and the mechanical performance of the coating can be improved.
Description
Technical field
The present invention relates to a kind of preparation method of nano particle, be specifically related to a kind of preparation method of protective system nano particle.
Background technology
In the exploitation of the reservoir such as oil, Sweet natural gas resource, exploitation, conveying, deposit process; in order to avoid the destruction that the corrosive medium in product causes hardware; cause equipment to be bored a hole and produce crack; people often carry out corrosion protection coating protection to its surface; to improve the working life of equipment, reduce because product leaks the harmful effect and financial loss caused environment.
Compactness is one of important indicator evaluating coating antiseptic performance.If the inside of coating or surface exist hole, corrosive medium easily arrives metal base surface by hole, corrosion reaction occurs on its surface and produces corrosion product.Corrosion product long-term accumulated, causes coating be full of cracks occurs and comes off, so that coating failure; Meanwhile, the existence of hole can reduce between coating and metal and between each layer of coating in conjunction with effect, affect the work-ing life of coating.
Nano particle, as a kind of small volume, new inorganic material that surface-area is larger, has the premium properties such as high strength, high tenacity, high thermal expansion coefficient differing from conventional material.Non-nano level filler traditional for its Some substitute is added in coating, can not only reduce costs, more can effectively improve coating compactness and corrosion resistance nature, improve wear resistance and the mechanical property of coating.But not a kind of concrete grammar prepared for coating nano particle specially in the market, for the development of nano paint provides theoretical foundation.
Summary of the invention
In order to solve above-mentioned prior art Problems existing, the object of the present invention is to provide a kind of preparation method of protective system nano particle, the size of nano particle is controlled by the potential of hydrogen of adjustment mother liquor system, thus realize the multistage composite of nano particle in dope preparing process, to improve compactness and the antiseptic property of nano coating.Meanwhile, in the preparation process of nano particle, add properties-correcting agent silane coupling agent, hydrophobic modification is carried out to the particle surface generated, improve its dispersiveness in coating, improve the physicochemical property on its surface.
In order to reach the above object, the present invention adopts following technical scheme:
A preparation method for protective system nano particle, comprises the steps:
Step 1: add metal alkoxide and dehydrated alcohol in the four-hole boiling flask that nitrogen protector, dropping funnel, agitator and thermometer are housed, makes system be warming up to 55 ~ 70 DEG C after stirring, form mother liquor; The mass ratio of described metal alkoxide and dehydrated alcohol is 1:(1.5 ~ 2);
Step 2: by the pH value of mother liquor in the hydrochloric acid of 1mol/L or sodium hydroxide solution regulating step 1 in 6 ~ 10 scopes, drip a certain amount of silane coupling agent, keep temperature to be 55 ~ 70 DEG C, stirring reaction 8 ~ 30 hours, until after system is hydrolyzed into the colloidal sol of homogeneous transparent, ageing becomes gel; The mass ratio of described silane coupling agent and metal alkoxide is (0 ~ 30): 100;
Step 3: with the product of dehydrated alcohol centrifuge washing step 2, constant temperature drying at 100 ~ 120 DEG C, is ground to white powder and is nano particle, is finally placed in vacuum drier sealing and preserves by nano particle.
Described metal alkoxide is tetraethoxy TEOS.
In described step 3, the nano particle diameter of preparation changes within the scope of 20 ~ 100nm.
Described silane coupling agent is dichlorodimethylsilane, KH-550 or KH-570.
The moistened surface contact angle of nano particle obtained in described step 3 changes within the scope of 0 ~ 130 °.
Compared to the prior art, the present invention has the following advantages:
(1) controllability of nano particle diameter can be realized by the pH value of adjustment mother liquor; The different nano particle of moistened surface degree can be obtained by the dosage changing silane coupling agent.
(2) owing to all having nitrogen protection in building-up process and stirring velocity is suitable for, the nano particle of final synthesis is the spherical of uniform particle sizes.
(3) the synthetic method energy consumption used is little, cost is low, operation is simple, is applicable to large-scale promotion and uses.
(4) composite by the nano particle of different-grain diameter, effectively can improve the compactness of inorganic-organic nanocomposite coating, improve the corrosion fatigue life of corrosion protection coating further.
Accompanying drawing explanation
Fig. 1 is the infrared spectrum contrast schematic diagram of rear nano grain surface before modified.
Fig. 2 is the SEM figure of different-grain diameter nano particle, and wherein Fig. 2 A is mean particle size be 60nm, Fig. 2 B be mean particle size be 48nm, Fig. 2 C be mean particle size is 27nm.
Fig. 3 is modified by nano particles front and rear surfaces hydrophobic rate test pattern.
Embodiment
Below in conjunction with embodiment, the present invention is described in further details.
Embodiment one
The preparation method of a kind of protective system nano particle of the present embodiment, is made up of the raw material of following mass percent: 36% tetraethoxy, 55% dehydrated alcohol, 7.8% hydrochloric acid soln (1mol/L), 1.2% dichlorodimethylsilane.
Prepare the protective system nano particle of the present embodiment, comprise the steps:
Step 1: add in the four-hole boiling flask that nitrogen protector, dropping funnel, agitator, thermometer are housed and account for all tetraethoxys of raw materials quality per-cent 36% and the dehydrated alcohol of 55%, be warming up to 65 DEG C after stirring.
Step 2: add the pH value of hydrochloric acid soln regulating step 1 solution accounting for all raw materials quality per-cent 7.8%, 1mol/L, drip the silane coupling agent accounting for all raw materials quality per-cent 1.2%, temperature is kept to be 65 DEG C, stirring reaction 18 hours, until after system is hydrolyzed into the colloidal sol of homogeneous transparent, ageing becomes gel.
Step 3: use dehydrated alcohol centrifuge washing product 3 times, constant temperature drying at 100 DEG C, is ground to white powder, is placed in vacuum drier sealing and preserves.
The nano particle median size of the method synthesis is 60nm (as shown in Figure 2 A), and grain diameter is even and better dispersed.And the silane coupling agent added in preparation process is successfully grafted on nano grain surface, make its surface have certain hydrophobicity, improve its dispersiveness in inorganic-organic nanocomposite coating.Be illustrated in figure 1 the infrared spectrum contrast adding the nano particle prepared before and after silane coupling agent.Nano particle modified as shown in Figure 3 all possesses certain hydrophobic oleophilic oil, and wherein a left side is unmodified nano particle, is all dispersed in aqueous phase; The right side is modified nano particle, is all dispersed in oil phase.
Embodiment two
The preparation method of a kind of protective system nano particle of the present embodiment, is made up of the raw material of following mass percent: 36% tetraethoxy, 55% dehydrated alcohol, 4% hydrochloric acid soln (1mol/L), 5% dichlorodimethylsilane.
Prepare the protective system nano particle of the present embodiment, comprise the steps:
Step 1: add in the four-hole boiling flask that nitrogen protector, dropping funnel, agitator, thermometer are housed and account for all tetraethoxys of raw materials quality per-cent 36% and the dehydrated alcohol of 55%, be warming up to 60 DEG C after stirring.
Step 2: the pH value adding hydrochloric acid soln regulating step 1 solution accounting for all raw materials quality per-cent 4%1mol/L, drip the silane coupling agent accounting for all raw materials quality per-cent 5%, temperature is kept to be 60 DEG C, stirring reaction 14 hours, until after system is hydrolyzed into the colloidal sol of homogeneous transparent, ageing becomes gel.
Step 3: use dehydrated alcohol centrifuge washing product 3 times, constant temperature drying at 110 DEG C, is ground to white powder, is placed in vacuum drier sealing and preserves.
The nano particle median size of the method synthesis is 48nm (as shown in Figure 2 B), and grain diameter is even and better dispersed.
Embodiment three
The preparation method of a kind of protective system nano particle of the present embodiment, is made up of the raw material of following mass percent: 36% tetraethoxy, 55% dehydrated alcohol, 2% hydrochloric acid soln (1mol/L), 7% dichlorodimethylsilane.
Prepare the protective system nano particle of the present embodiment, comprise the steps:
Step 1: add in the four-hole boiling flask that nitrogen protector, dropping funnel, agitator, thermometer are housed and account for all tetraethoxys of raw materials quality per-cent 36% and the dehydrated alcohol of 55%, be warming up to 55 DEG C after stirring.
Step 2: the pH value adding hydrochloric acid soln regulating step 1 solution accounting for all raw materials quality per-cent 2%1mol/L, drip the silane coupling agent accounting for all raw materials quality per-cent 7%, temperature is kept to be 55 DEG C, stirring reaction 12 hours, until after system is hydrolyzed into the colloidal sol of homogeneous transparent, ageing becomes gel.
Step 3: use dehydrated alcohol centrifuge washing product 3 times, constant temperature drying at 120 DEG C, is ground to white powder, is placed in vacuum drier sealing and preserves.
The nano particle median size of the method synthesis is 27nm (as shown in Figure 2 C), and grain diameter is even and better dispersed.
Claims (5)
1. a preparation method for protective system nano particle, is characterized in that: comprise the steps:
Step 1: add metal alkoxide and dehydrated alcohol in the four-hole boiling flask that nitrogen protector, dropping funnel, agitator and thermometer are housed, makes system be warming up to 55 ~ 70 DEG C after stirring, form mother liquor; The mass ratio of described metal alkoxide and dehydrated alcohol is 1:(1.5 ~ 2);
Step 2: by the pH value of mother liquor in the hydrochloric acid of 1mol/L or sodium hydroxide solution regulating step 1 in 6 ~ 10 scopes, drip a certain amount of silane coupling agent, keep temperature to be 55 ~ 70 DEG C, stirring reaction 8 ~ 30 hours, until after system is hydrolyzed into the colloidal sol of homogeneous transparent, ageing becomes gel; The mass ratio of described silane coupling agent and metal alkoxide is (0 ~ 30): 100;
Step 3: with the product of dehydrated alcohol centrifuge washing step 2, constant temperature drying at 100 ~ 120 DEG C, is ground to white powder and is obtained nano particle, is finally placed in vacuum drier sealing and preserves by nano particle.
2. the preparation method of a kind of protective system nano particle according to claim 1, is characterized in that: described metal alkoxide is tetraethoxy TEOS.
3. the preparation method of a kind of protective system nano particle according to claim 1, is characterized in that: in described step 3, the nano particle diameter of preparation changes within the scope of 20 ~ 100nm.
4. the preparation method of a kind of protective system nano particle according to claim 1, is characterized in that: described silane coupling agent is dichlorodimethylsilane, KH-550 or KH-570.
5. the preparation method of a kind of protective system nano particle according to claim 1, is characterized in that: the moistened surface contact angle of nano particle obtained in described step 3 changes within the scope of 0 ~ 130 °.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106047000A (en) * | 2016-08-20 | 2016-10-26 | 哈尔滨锅炉厂有限责任公司 | Hydraulic pressure anti-rust agent for boiler auxiliary machine container products, and preparation method thereof |
| CN110079181A (en) * | 2019-04-12 | 2019-08-02 | 西安理工大学 | A kind of preparation method of environmental response type super-amphiphobic coating |
| CN113053651A (en) * | 2021-03-24 | 2021-06-29 | 福建尚辉润德新材料科技有限公司 | Preparation method of soft magnetic composite material and soft magnetic composite material |
| CN113248190A (en) * | 2016-06-02 | 2021-08-13 | 纳米及先进材料研发院有限公司 | Super-flexible nano modified polymer cement-based waterproof coating and preparation method thereof |
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| CN101704529A (en) * | 2009-11-05 | 2010-05-12 | 西北工业大学 | Method for preparing amphiphilic nano silica powder and method for preparing Pickering emulsion using same |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113248190A (en) * | 2016-06-02 | 2021-08-13 | 纳米及先进材料研发院有限公司 | Super-flexible nano modified polymer cement-based waterproof coating and preparation method thereof |
| CN106047000A (en) * | 2016-08-20 | 2016-10-26 | 哈尔滨锅炉厂有限责任公司 | Hydraulic pressure anti-rust agent for boiler auxiliary machine container products, and preparation method thereof |
| CN110079181A (en) * | 2019-04-12 | 2019-08-02 | 西安理工大学 | A kind of preparation method of environmental response type super-amphiphobic coating |
| CN113053651A (en) * | 2021-03-24 | 2021-06-29 | 福建尚辉润德新材料科技有限公司 | Preparation method of soft magnetic composite material and soft magnetic composite material |
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Application publication date: 20151125 |