CN116103658B - Gas-phase antirust hair dispersion suitable for multiple metals and preparation method thereof - Google Patents
Gas-phase antirust hair dispersion suitable for multiple metals and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F11/00—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent
- C23F11/02—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in air or gases by adding vapour phase inhibitors
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Abstract
The invention discloses a gas-phase rust-proof dispersion suitable for multiple metals, which comprises the following components in percentage by mass: 25-35% of benzotriazole, 20-30% of dimethyl imidazole and 12-25% of span 40 (sorbitan monopalmitate); further comprises: 8-10% of sodium citrate, 4-8% of water-based lanolin, 4-8% of sodium dodecyl benzene sulfonate and 4-8% of additive. The invention solves the problem that the existing gas-phase rust-proof powder can not meet the requirement of multi-metal protection at the same time. The invention also provides a preparation method of the gas-phase rust-proof hair dispersion.
Description
Technical Field
The invention relates to the technical field of gas-phase rust prevention, in particular to a gas-phase rust prevention dispersion suitable for multiple metals and a preparation method thereof.
Background
Electrical equipment has high corrosion control requirements and slight corrosion can affect its performance. In marine environment, the conditions are bad, and the used electronic and electric equipment contains various metal materials, especially if corrosion control measures such as metal screws, wiring terminals, connectors, circuit board through holes and the like are improper, early corrosion problems are easy to occur, and hidden dangers are buried for subsequent operation of products.
The gas-phase rust prevention technology has the advantages of no limitation on the shape of equipment and no hole and can protect metal equipment, and is widely applied to industries such as workshop storage, packaging and transportation, and the like, and the protection effect of the gas-phase rust prevention technology is widely accepted by the industries. However, for metal gas-phase rust prevention, single metal gas-phase rust prevention products are mainly used in the market at present, but due to various metal materials involved in electronic and electric appliances, the single metal gas-phase rust prevention products cannot meet multi-metal rust prevention requirements, and different types of rust prevention products may have the problem of incompatibility in rust prevention.
In addition, the gas phase rust-preventive material is morphologically mainly divided into powder and liquid; gaseous rust-preventive liquids such as rust-preventive oil, which are liable to stain electronic components after leakage; in contrast, the gas-phase rust-proof powder solves the leakage problem, is more suitable for rust prevention of electronic and electric appliances, but is easy to agglomerate in a humid environment, and can cause poor rust prevention effect.
Therefore, there is a strong need to develop a gas-phase rust-preventing powder which is suitable for multiple metals, has high efficiency, multiple occasions and less agglomeration, and ensures the safe operation of electronic and electrical equipment and the safety of users.
Disclosure of Invention
The invention aims to provide a gas-phase rust-proof dispersion suitable for multiple metals and a preparation method thereof, and solves the problem that the existing gas-phase rust-proof powder cannot meet the protection requirement of multiple metals at the same time.
In order to achieve the above purpose, the present invention adopts the following scheme:
the gas-phase rust-proof dispersion suitable for the multi-metal comprises the following components in percentage by mass: 25-35% of benzotriazole, 20-30% of dimethyl imidazole and 12-25% of span 40 (sorbitan monopalmitate).
The invention discovers that span 40 plays an anti-rust role on copper, zinc, steel and aluminum metals, and the molecular structure analysis deduces that as one side of the molecular structure of the span comprises a long alkyl branched chain and the other side of the molecular structure is provided with a hydrophilic group, the hydrophilic group is adsorbed and forms a compact hydrophobic film on the surface of the metals, and the alkyl branched chain is further used for blocking moisture, oxygen and metal contact, so that corrosion inhibition is effectively realized. And the combination of benzotriazole, dimethylimidazole and span 40 screened by electrochemical compounding has good antirust performance on copper, zinc, steel and aluminum.
As a further aspect of the invention:
the span 40 is a porous span 40 skeleton with a skeleton structure, and the specific preparation method comprises the following steps: fully dispersing span 40 in deionized water by utilizing ultrasonic action to form white uniform emulsion; then adding superfine iron powder, continuing to carry out ultrasonic treatment, uniformly dispersing, and then carrying out quick vacuum freeze drying; grinding and sieving the superfine iron powder-span 40 mixed solid; and finally, soaking the mixed solid in dilute acid, filtering, repeatedly washing with water to neutrality, and drying to obtain the porous span 40 skeleton.
Aiming at the problem that the existing gas-phase rust-proof powder is easy to agglomerate due to the fact that the effective radiating surface area of the particles is too large, the invention provides a porous skeleton made of span 40 which is one of rust-proof components, the agglomeration of the powder is reduced by using the porous skeleton support, and the porous structure can absorb trace water vapor in the environment, so that the rust-proof effect of the product is improved.
As a further aspect of the invention:
the gas-phase antirust dispersion comprises the following components in percentage by mass: 8-10% of sodium citrate, 4-8% of water-based lanolin, 4-8% of sodium dodecyl benzene sulfonate and 4-8% of additive; the additive is mildew inhibitor and adsorptivity auxiliary agent.
The invention also provides a preparation method of the gas-phase rust-proof dispersion, which comprises the following steps: and mixing the components in proportion, and then fully grinding and sieving to obtain the gas-phase rust-proof dispersion.
In the process of the invention, the components are ground to pass through a 500-1000 mesh screen.
As a further aspect of the invention: before the components are mixed, the span 40 is made into a porous span 40 framework, and the specific steps are as follows: (1) Fully dispersing span 40 in deionized water by utilizing ultrasonic action to form white uniform emulsion; (2) Then adding superfine iron powder, continuing to carry out ultrasonic treatment, uniformly dispersing, and then carrying out quick vacuum freeze drying to obtain superfine iron powder-span 40 mixed solid; (3) Grinding and sieving the superfine iron powder-span 40 mixed solid to obtain mixed powder; (4) And finally, soaking the mixed powder obtained in the step (3) in dilute acid, filtering, repeatedly washing with water to neutrality, and drying to obtain the porous span 40 skeleton.
Further, the porous span 40 skeleton is mixed with other components in the following manner: the porous span 40 skeleton and other components which are ground and sieved by a 500-1000-mesh sieve are placed in a three-neck flask for vacuum dispersion, so that the other components are attached to the skeleton, and the gas-phase antirust dispersing body applicable to multiple metals is prepared.
In step (1), the ratio of span 40 to deionized water is 1g:2.5ml; the ultrasound time was 2h.
In the step (1), deionized water is subjected to deoxidization treatment, specifically: introducing N into deionized water 2 An inert gas; the deoxidizing treatment is to ensure that the iron powder is not oxidized, so that the skeleton of the porous span 40 reaches a good aperture state.
In the step (2), the grain size of the superfine iron powder is 2-5 mu m; the mass ratio of span 40 to superfine iron powder is 1:0.5-1.
In the step (3), the superfine iron powder-span 40 mixed solid is ground in a mortar, and then passes through a 100-mesh screen and then a 150-mesh screen, and mixed powder between 100 and 150 meshes is reserved.
In the step (3), the superfine powder is continuously ground, the superfine iron powder is sucked away by the magnet, and the rest span 40 can be continuously used as a raw material for manufacturing the porous framework.
In the step (4), the mixed powder is soaked in dilute acid at low temperature, then repeatedly washed to be neutral by ice water, dried, and then checked for the residual condition of iron powder by a magnet, and finally the porous span 40 skeleton is obtained.
The invention also provides the gas-phase rust-proof dispersion which is suitable for multiple metals and is prepared by the method.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the invention, the combination of benzotriazole, dimethylimidazole and span 40 is screened out through electrochemical compounding, so that the rust prevention of copper, zinc, steel and aluminum components is realized, the problem that the existing gas-phase rust prevention powder cannot meet the requirement of multi-metal protection at the same time is solved, and the problem of multi-metal rust prevention compatibility is avoided.
2. The invention utilizes the skeleton structure of the porous span 40 to increase the effective surface area of the rust-proof component, which is beneficial to the dispersion of the rust-proof component, and simultaneously utilizes the skeleton structure to load finer powder, thereby reducing the problem of massive agglomeration and ensuring that the rust-proof powder protects metals better.
Drawings
Fig. 1 is a graph showing the polarization curves of the components in four different metals after being compounded in the first example.
Detailed Description
The invention is further illustrated in detail below in conjunction with specific examples, which are provided solely for the purpose of illustrating the invention and are not intended to limit the scope of the invention. The test methods used in the following examples are conventional methods unless otherwise specified; the materials, reagents and the like used, unless otherwise specified, are those commercially available.
Example 1
The testing method of the rust-proof effect comprises the following steps:
1) Atmospheric corrosion simulation liquid preparation: preparation of analytical pure NaHCO containing 100mg/L Using deionized Water 3 、Na 2 SO 4 Solution of NaCl;
2) Preparing an antirust liquid: preparing a gas-phase antirust component solution containing 1g/L by using the atmospheric corrosion simulation solution as a base solution;
3) Preparing steel, copper, zinc and aluminum test electrodes: soldering a 1cm x 1cm metal sheet to a wire and encapsulating the wire with epoxy resin to form an exposed area of 1cm x 1cm;
4) Performance test: three electrodes are adopted for testing, antirust liquid is used as electrolyte, steel, copper, zinc and aluminum with the exposure area of 1cm x 1cm are used as working electrodes, a platinum sheet electrode with the exposure area of 1cm x 1cm is used as an auxiliary electrode, and an Ag/AgCl electrode is used as a reference electrode. Polarization curve test potential scan range + -250 mV (vs OCP), scan speed 0.005V/s, all electrochemical tests were performed at normal temperature.
5) Data analysis: drawing an E-log|i|image, performing data analysis by mainly using a tafel curve to perform tangent fitting at an equilibrium potential of +/-60 mV, intersecting cathode and anode tangents, intersecting an intersection point with an elongation line of the lowest point of the tafel curve, wherein the potential corresponding to the intersection point is a self-corrosion potential, the current is a self-corrosion current, and the corrosion inhibition rate calculating method comprises the following steps:
the self-corrosion potential represents the corrosion trend of metal, and generally, the greater the self-corrosion potential is, the more difficult the corrosion is, the data only make preliminary trend judgment, and the performance comparison is mainly based on the self-corrosion current. While the self-etching current indicates the metal rate, the greater the self-etching current, the faster the metal is etched. The performance of the gas-phase rust-proof component is evaluated mainly by using corrosion inhibition efficiency, and the calculation formula is as follows:
wherein, eta: corrosion inhibition rate;
i0: corrosion current density of metal without gas phase rust preventive component;
i1: corrosion current of metal added with gas phase rust-proof component
1. And (3) testing the rust-proof effect of each component: rust-preventive solutions containing 1g/L benzotriazole, dimethylimidazole, span 40, sodium citrate, aqueous lanolin and sodium dodecylbenzenesulfonate were prepared, and steel, copper, zinc and aluminum were tested for rust-preventive effect according to the above-described method, and the results are shown in table 1.
TABLE 1
The data analysis in table 1 shows that dimethylimidazole and sodium citrate have obvious corrosion inhibition effect on steel, benzotriazole has obvious corrosion inhibition effect on copper and zinc, span 40 has obvious corrosion inhibition effect on aluminum, and the compounding is used for obtaining the optimal corrosion inhibition efficiency of each metal through the synergistic effect, so that the problem of incompatibility in rust prevention is avoided. The data analysis shows that benzotriazole has a slight negative corrosion inhibition effect on aluminum, but has a good corrosion inhibition effect on other components, especially copper and zinc corrosion inhibition efficiency is over 95 percent, so that benzotriazole is used as a main rust-proof component, the rust-proof performance of steel and aluminum is improved by compounding, the corrosion inhibition effect of dimethylimidazole in the steel is better, and the negative effects of the other three metals are smaller than those of sodium citrate.
Note that: the non-rust component directly takes the atmosphere simulation liquid as electrolyte, no rust component is added, and other testing processes are consistent with the addition of the rust component.
2. And (3) testing the rust-proof effect of the compound combination of the components with different proportions: the rust preventive solutions of combinations 1 to 3 were prepared according to the proportions shown in Table 1, and the rust preventive solution was prepared as follows (taking the rust preventive solution of combination 1 as an example):
2g of benzotriazole, 1.9g of dimethyl imidazole, 0.8g of span 40, 0.6g of sodium citrate, 0.5g of aqueous lanolin and 0.5g of sodium dodecyl benzene sulfonate are respectively weighed, and are fully dissolved by using an atmospheric corrosion simulation solution to prepare 1L solution;
the rust preventive effect of the rust preventive liquid on steel, copper, zinc, aluminum was tested according to the above method, and the results are shown in table 2 and fig. 1.
TABLE 2
The results in tables 1-2 and fig. 1 demonstrate that although benzotriazole, dimethylimidazole, span 40 sodium citrate, aqueous lanolin and sodium dodecylbenzenesulfonate have positive or negative rust inhibiting effects on different metals, the components, after being compounded, all have positive rust inhibiting effects on steel, copper, zinc, aluminum by synergistic action.
Example two preparation of gas phase rust inhibitive divergents suitable for Multimetals
(1) Preparing a porous span 40 skeleton:
(1a) Weighing 20g of span 40 (sorbitan monopalmitate), adding into 50mL of deionized water subjected to deoxidization treatment, and dispersing in ultrasonic for 2 hours to form white uniform emulsion;
(1b) Adding 20g of superfine iron powder with the particle size of 2-5 mu m, continuing to carry out ultrasonic treatment, uniformly dispersing, and then carrying out quick vacuum freeze drying to obtain superfine iron powder-span 40 mixed solid;
(1c) Grinding the superfine iron powder-span 40 mixed solid in a mortar, sieving with a 100-mesh sieve, sieving with a 150-mesh sieve, and reserving mixed powder with the particle size of between 100 and 150 mu m;
continuously grinding the superfine powder, and sucking away the superfine iron powder by using a magnet to obtain the rest span 40 which can be continuously used as a raw material for manufacturing the porous framework;
(1d) Soaking the reserved mixed powder in 0.5mol of dilute hydrochloric acid at 10 ℃ for 24 hours, filtering, repeatedly washing with ice water to neutrality, and checking the residue of iron powder by using a magnet to obtain a porous span 40 skeleton;
note that: span 40 is dissolved in hot water and to avoid collapse or dissolution of the scaffold, the scaffold should be prepared in a solution at a temperature below 20 ℃.
(2) Preparing a gas phase rust-proof dispersion suitable for multiple metals:
(2a) Weighing 0.7g of benzotriazole, 0.5g of dimethyl imidazole, 0.2g of sodium citrate, 0.1g of aqueous lanolin, 0.1g of sodium dodecyl benzene sulfonate and 0.1g of adsorptivity aid (specifically hexamethylenetetramine), mixing, and grinding until the mixture passes through a 1000-mesh screen (the particle size is smaller than 15 mu m) to obtain mixed micro powder;
(2b) Weighing 0.3g of porous span 40 skeleton, placing the porous span 40 skeleton and the mixed micro powder in a three-necked flask, connecting a vacuum pump, and performing vacuum dispersion to enable powder to be attached to the skeleton, thus preparing the gas-phase rust-proof dispersion suitable for multiple metals.
EXAMPLE three preparation of gas phase rust inhibitive divergents suitable for Multimetals
(1) Preparing a porous span 40 skeleton:
(1a) Weighing 20g of span 40 (sorbitan monopalmitate), adding into 50mL of deionized water subjected to deoxidization treatment, and dispersing in ultrasonic for 2 hours to form white uniform emulsion;
(1b) Adding 10g of superfine iron powder with the particle size of 2-5 mu m, continuing to carry out ultrasonic treatment, uniformly dispersing, and then carrying out quick vacuum freeze drying to obtain superfine iron powder-span 40 mixed solid;
(1c) Grinding the superfine iron powder-span 40 mixed solid in a mortar, sieving with a 100-mesh sieve, sieving with a 150-mesh sieve, and reserving mixed powder with the particle size of between 100 and 150 mu m;
continuously grinding the superfine powder, and sucking away the superfine iron powder by using a magnet to obtain the rest span 40 which can be continuously used as a raw material for manufacturing the porous framework;
(1d) Soaking the reserved mixed powder in 0.5mol of dilute hydrochloric acid at 10 ℃ for 24 hours, filtering, repeatedly washing with ice water to neutrality, and checking the residue of iron powder by using a magnet to obtain a porous span 40 skeleton;
(2) Preparing a gas phase rust-proof dispersion suitable for multiple metals:
(2a) Weighing 0.7g of benzotriazole, 0.6g of dimethyl imidazole, 0.15g of sodium citrate, 0.2g of aqueous lanolin, 0.1g of sodium dodecyl benzene sulfonate and 0.1g of adsorptivity aid (specifically hexamethylenetetramine), mixing, and grinding until the mixture passes through a 500-mesh screen (the particle size is smaller than 30 mu m) to obtain mixed micro powder;
(2b) Weighing 0.4g of porous span 40 skeleton, placing the porous span 40 skeleton and the mixed micro powder in a three-necked flask, connecting a vacuum pump, and performing vacuum dispersion to enable powder to be attached to the skeleton, thus preparing the gas-phase rust-proof dispersion suitable for multiple metals.
The present invention may be summarized in other specific forms without departing from the spirit or essential characteristics thereof. The above-described embodiments of the present invention are to be considered in all respects only as illustrative and not restrictive. Therefore, any minor modifications, equivalent changes and modifications made to the above embodiments according to the essential technology of the present invention fall within the scope of the present invention.
Claims (9)
1. The gas-phase rust-proof dispersion suitable for the multi-metal is characterized by comprising the following components in percentage by mass: 25-35% of benzotriazole, 20-30% of dimethyl imidazole and 40-25% of span;
wherein, span 40 is porous span 40 skeleton with skeleton structure, the concrete preparation method is: fully dispersing span 40 in deionized water by utilizing ultrasonic action to form white uniform emulsion; then adding superfine iron powder, continuing to carry out ultrasonic treatment, uniformly dispersing, and then carrying out quick vacuum freeze drying; grinding and sieving the superfine iron powder-span 40 mixed solid; and finally, soaking the mixed solid in dilute acid, filtering, repeatedly washing with water to neutrality, and drying to obtain the porous span 40 skeleton.
2. The gas phase rust inhibitive hair dispersion according to claim 1, further comprising, in mass ratio: 8-10% of sodium citrate, 4-8% of aqueous lanolin, 4-8% of sodium dodecyl benzene sulfonate and 4-8% of additives; the additive is mildew inhibitor and adsorptivity auxiliary agent.
3. A method for producing the gas phase rust inhibitive hair dispersion according to claim 1 or 2, comprising the steps of: and mixing the components in proportion, and then fully grinding and sieving to obtain the gas-phase rust-proof dispersion.
4. The preparation method according to claim 3, wherein the porous span 40 skeleton is prepared from span 40 before mixing the components, and the specific steps are as follows: (1) Fully dispersing span 40 in deionized water by utilizing ultrasonic action to form white uniform emulsion; (2) Then adding superfine iron powder, continuing to carry out ultrasonic treatment, uniformly dispersing, and then carrying out quick vacuum freeze drying to obtain superfine iron powder-span 40 mixed solid; (3) Grinding and sieving the superfine iron powder-span 40 mixed solid to obtain mixed powder; (4) And finally, soaking the mixed powder obtained in the step (3) in dilute acid, filtering, repeatedly washing with water to neutrality, and drying to obtain the porous span 40 skeleton.
5. The method according to claim 4, wherein in the step (1), the ratio of span 40 to deionized water is 1 g/2.5 ml and the ultrasonic time is 2 hours; the deionized water is subjected to deoxidization treatment, and specifically comprises the following steps: introducing N into deionized water 2 An inert gas.
6. The method according to claim 4, wherein in the step (2), the particle size of the ultrafine iron powder is 2 to 5 μm; the mass ratio of span 40 to superfine iron powder is 1:0.5-1.
7. The method according to claim 6, wherein in the step (3), the ultrafine iron powder-span 40 mixed solid is ground in a mortar, and then passes through a 100-mesh screen and then a 150-mesh screen, and the mixed powder of 100-150 mesh is retained.
8. The method according to claim 7, wherein in the step (4), the mixed powder is immersed in dilute acid at a low temperature, then repeatedly washed with ice water to neutrality, dried, and then inspected for residual iron powder by a magnet, thereby obtaining the porous span 40 skeleton.
9. The preparation method of claim 8, wherein the porous span 40 skeleton is mixed with other components in the following manner: and placing the porous span 40 framework and other components which are ground and sieved by a 500-1000-mesh sieve into a three-neck flask, and performing vacuum dispersion to enable the other components to be attached to the framework, so as to prepare the gas-phase rust-proof dispersion suitable for multiple metals.
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