CN114369828B - Aluminum alloy acid etching solution and preparation method thereof - Google Patents
Aluminum alloy acid etching solution and preparation method thereof Download PDFInfo
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- 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
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Abstract
The application relates to the field of acid etching solutions, and particularly discloses an aluminum alloy acid etching solution and a preparation method thereof. The aluminum alloy acid etching solution comprises the following components in parts by mass: 48-50 parts of nitric acid; 24-25 parts of sulfuric acid; 5-6 parts of ammonium bifluoride; 0-1 part of degreasing agent; 18-23 parts of water; the total mass fraction is 100. The preparation method comprises the following steps: step 1), water is injected into a container, sulfuric acid is added into the water, and stirring and cooling are carried out to room temperature, so as to obtain sulfuric acid solution; step 2), adding nitric acid into the sulfuric acid solution, stirring and cooling to room temperature to obtain a mixed solution; and 3) adding ammonium bifluoride and degreasing agent into the mixed solution, and uniformly stirring to obtain the aluminum alloy acid etching solution. The application has the effects of improving the acid etching efficiency and keeping the aluminum material to have better quality.
Description
Technical Field
The application relates to the field of acid etching solutions, in particular to an aluminum alloy acid etching solution and a preparation method thereof.
Background
The aluminum alloy is an alloy prepared by taking aluminum as a base material and adding a certain amount of other alloying elements, and is one of light metal materials.
In order to improve the corrosion resistance and weather resistance of the aluminum alloy material, the surface of the aluminum alloy material is usually required to be sprayed for protection, the surface of the aluminum alloy is required to be kept clean before spraying, grease and impurities on the surface are required to be removed, so that the coating is tightly attached to the aluminum alloy, and the peeling phenomenon is not easy to occur.
The existing degreasing treatment of the aluminum alloy surface mainly comprises alkali corrosion and acid corrosion, and the alkali corrosion is slow in reaction and easy to generate coarse crystal phenomenon, so that the acid corrosion technology gradually occupies the main stream.
The aluminum material acid etching needs to adopt acid etching liquid, sulfuric acid is one of the main components of the acid etching liquid, sulfuric acid can dissolve and strip natural oxide films formed on the surface of the aluminum alloy, and can play a role in activating the surface of the aluminum material, when the sulfuric acid concentration is too high, the corrosion speed of the aluminum is higher, over corrosion is easy to generate, and the brightness is reduced, so that the sulfuric acid concentration in the general acid etching liquid is not more than 15 percent.
However, the concentration of sulfuric acid is related to the reaction speed, in order to avoid excessive corrosion caused by too high speed, the concentration of sulfuric acid is low, so that the acid corrosion needs longer, usually 1-5min is needed, the efficiency is still lower although the acid corrosion is faster than the alkali corrosion, if the efficiency is improved simply by increasing the concentration of sulfuric acid, excessive corrosion is easy to occur because the acid corrosion time is difficult to control, and the quality of aluminum products is reduced, so that the improvement room is left.
Disclosure of Invention
The application provides an aluminum alloy acid etching solution and a preparation method thereof in order to improve the acid etching efficiency and keep the aluminum material to have better quality.
In a first aspect, the application provides an aluminum alloy acid etching solution, which adopts the following technical scheme:
the aluminum alloy acid etching solution comprises the following components in parts by mass:
48-50 parts of nitric acid;
24-25 parts of sulfuric acid;
5-6 parts of ammonium bifluoride;
0-1 part of degreasing agent;
18-23 parts of water;
the total mass fraction is 100.
Preferably, the composition comprises the following components in parts by weight:
48.5-49.5 parts of nitric acid;
24.25-24.75 parts of sulfuric acid;
5.25-5.75 parts of ammonium bifluoride;
0-1 part of degreasing agent;
19.25-21.75 parts of water;
the total mass fraction is 100.
By adopting the technical scheme, the acid etching speed is greatly improved by the concentration of sulfuric acid reaching 24% -25%, according to the actual condition of the aluminum product, the acid etching can be basically finished within 3s-30s, as the acid etching speed is higher, nitric acid with the concentration reaching 48% -50% is added for the proportion over-etching phenomenon, nitric acid is a strong oxidant, and after the natural maintenance film on the surface of the aluminum product is corroded by sulfuric acid, a brand-new and compact aluminum oxide passivation film can be generated under the action of nitric acid due to the higher nitric acid content, the corrosion prevention effect of the aluminum oxide passivation film is excellent, the higher sulfuric acid etching speed is restrained, so that the acid etching efficiency is improved, but once grease and impurities attached to the surface of the aluminum product are stripped due to the acid etching, the aluminum product surface can be quickly formed into the aluminum oxide passivation film to protect the aluminum product, the aluminum product is not easy to be quickly corroded by the acid etching agent, the aluminum product is not easy to stay for a long time, the over-etching cannot be caused, the condition of being reduced can not occur, the aluminum product can be quickly corroded by the acid etching agent, and the aluminum product can be kept in the good quality for the aluminum product to be quickly etched, and the aluminum product can be simultaneously buffered, and the quality of the aluminum product can be maintained.
The addition of ammonium bifluoride can accelerate the dissolution of a natural oxide film on the surface of aluminum, eliminate or reduce defects such as indentation and the like, so that the surface of aluminum is smooth and clean, and has stronger complexing capability, elements such as manganese, copper, silicon and the like on the surface of aluminum alloy can be dissolved, so that a black film is not easy to appear on the surface of aluminum alloy, the brightness of aluminum alloy is better, meanwhile, fluorine element can accelerate the formation of an aluminum oxide passivation film, and nitric acid is assisted to enable the clean surface of aluminum alloy to quickly form the aluminum oxide passivation film so as to prevent further corrosion of sulfuric acid, so that the acid etching efficiency is higher and the harm of over-corrosion is not easy to appear.
Preferably, the degreasing agent is a compound of ferrous sulfate, dipropylene glycol and a nonionic surfactant.
Through adopting above-mentioned technical scheme, through ferrous sulfate's addition, under the strong oxidation of nitric acid, produce ferric ion, ferric ion can take place the displacement reaction on aluminum alloy surface, forms micro-cell for aluminum alloy surface produces trace hydrogen, makes the greasy dirt more easily leave aluminum alloy surface through hydrogen, accelerates degreasing effect.
Through the cooperation of dipropylene glycol and nonionic surfactant, the solubility of grease in acid etching is greatly increased, grease is not easy to attach to the surface of aluminum alloy after falling off, the surface of the aluminum alloy after acid etching is finished is cleaner, the service life of acid etching liquid is longer, more aluminum alloy materials can be treated, the frequency of changing the acid etching liquid is reduced, and the method has higher economic value.
Preferably, the mass ratio of the ferrous sulfate, the dipropylene glycol and the nonionic surfactant is 1:0.2:0.3.
through adopting above-mentioned technical scheme, through selecting the specific proportion to compound for degreasing effect is better, and speed is faster, more helps improving acid etching efficiency.
Preferably, the nonionic surfactant is a compound of alkylphenol ethoxylates and fatty alcohol ethoxylates.
Through adopting above-mentioned technical scheme, through adopting alkylphenol ethoxylate, fatty alcohol ethoxylate to compound, be the solubility to the grease stronger, the grease is dissolved and drops with higher speed, and makes the difficult adhesion again of grease on aluminum alloy, degreasing effect is better.
Preferably, the mass ratio of the alkylphenol ethoxylates to the fatty alcohol ethoxylates is 1:1.
through adopting above-mentioned technical scheme, through selecting specific proportion cooperation for degreasing effect is better, and acid etching efficiency is higher, and the limit of acid etching liquid dissolved grease is higher, and life is longer.
In a second aspect, the application provides a preparation method of an aluminum alloy acid etching solution, which adopts the following technical scheme:
the preparation method of the aluminum alloy acid etching solution comprises the following steps:
step 1), water is injected into a container, sulfuric acid is added into the water, and stirring and cooling are carried out to room temperature, so as to obtain sulfuric acid solution;
step 2), adding nitric acid into the sulfuric acid solution, stirring and cooling to room temperature to obtain a mixed solution;
and 3) adding ammonium bifluoride and degreasing agent into the mixed solution, and uniformly stirring to obtain the aluminum alloy acid etching solution.
Through adopting above-mentioned technical scheme, through stirring cooling, reduce the temperature of acid etching liquid, because the content of concentrated acid is higher, if add too fast, arouse boiling easily and lead to acid to spill, lead to the fact the incident easily, can make exothermic influence obtain reducing by a wide margin through stirring cooling, improve production safety.
Preferably, in the step 1), when sulfuric acid is added to the water, the sulfuric acid is injected at a constant speed for 10min, and in the step 2), when nitric acid is added to the sulfuric acid solution, the nitric acid is injected at a constant speed for 15min.
By adopting the technical scheme, the concentrated accumulation of heat in the exothermic process is further reduced by controlling the injection time of the acid, so that the production safety is higher in the process of preparing the acid etching solution.
In summary, the application has the following beneficial effects:
1. according to the application, the acid etching speed is greatly improved by the concentration of sulfuric acid reaching 24% -25%, and according to the actual condition of the aluminum material, the acid etching can be basically finished within 3s-30s, and due to the fact that the acid etching speed is higher, nitric acid with the concentration reaching 48% -50% is added for the over-etching phenomenon of proportion, and is a strong oxidant, and due to the fact that the nitric acid content is higher, after the natural maintenance film on the surface of the aluminum material is corroded by sulfuric acid, a brand-new and compact aluminum oxide passivation film can be generated under the action of nitric acid, the corrosion prevention effect of the aluminum oxide passivation film is excellent, so that the corrosion prevention speed of the sulfuric acid with the higher concentration is restrained, and the acid etching efficiency is improved, but once grease and impurities attached to the surface of the aluminum material are stripped due to the acid etching, the aluminum material surface can be rapidly formed to protect the aluminum material, the aluminum material is not rapidly corroded, the aluminum material is not easily corroded rapidly, the aluminum material is not subjected to multiple light brightness stay for a period of time, the over-etching is not caused, the condition that the corrosion is not reduced is not caused, the aluminum material can be rapidly corroded in the acid agent, and the good quality is maintained, and the aluminum material can be well buffered.
2. According to the application, the natural oxide film on the aluminum surface can be accelerated and dissolved by adding ammonium bifluoride, defects such as indentation and the like are eliminated or reduced, so that the aluminum surface is smooth and clean, the complex capability is high, elements such as manganese, copper, silicon and the like on the aluminum alloy surface and impurities can be dissolved, so that a black film is not easy to appear on the aluminum alloy surface, the brightness of the aluminum alloy is better, meanwhile, the fluorine element can accelerate the formation of an aluminum oxide passivation film, and the clean aluminum alloy surface is enabled to quickly form the aluminum oxide passivation film by assisting nitric acid so as to prevent further corrosion of sulfuric acid, so that the acid etching efficiency is high and the harm of over-corrosion is not easy to appear.
3. According to the application, the solubility of grease in acid etching is greatly increased by matching dipropylene glycol with the nonionic surfactant, so that grease is not easy to attach to the surface of aluminum alloy after being removed, the surface of the aluminum alloy after acid etching is cleaner, the service life of acid etching liquid is longer, more aluminum alloy materials can be treated, the frequency of changing the acid etching liquid is reduced, and the method has higher economic value.
4. According to the method, the temperature of the acid etching solution is reduced through stirring and cooling, and the concentrated acid is high in content, so that if the concentrated acid is added too quickly, the acid is easy to splash due to boiling, safety accidents are easy to cause, the influence of heat release can be greatly reduced through stirring and cooling, and the production safety is improved.
Detailed Description
The present application will be described in further detail with reference to examples.
The source information of the raw materials used in the following examples and comparative examples is shown in Table 1.
TABLE 1
| Source information | |
| Nitric acid | Concentrated nitric acid, 98% concentration, of Jinan Ying Chemicals Limited |
| Sulfuric acid | Concentrated sulfuric acid with concentration of 98% in the MaoMing market and Male chemical industry limited formula |
| Ammonium bifluoride | Wuhan Rabdosia science and technology Co., ltd., CAS:1341-49-7 |
| Ferrous sulfate | Shandong Qing Yixin chemical engineering Co., ltd., CAS:7782-63-0 |
| Dipropylene glycol | Aite (Shandong) New Material Co., ltd., CAS110-98-5 |
| Alkylphenol polyoxyethylene | Emulsifier OP-10, of Jinan Hongshun chemical Co., ltd |
| Fatty alcohol polyoxyethylene ether | Emulator AEO-9, jinan Maifeng chemical Co., ltd |
Examples 1 to 5
An aluminum alloy acid etching solution comprises the following components:
nitric acid, sulfuric acid, ammonium bifluoride, degreasing agent and water.
Wherein the degreasing agent is a compound of ferrous sulfate, dipropylene glycol and a nonionic surfactant, and the mass ratio of the ferrous sulfate to the dipropylene glycol to the nonionic surfactant is 1:0.2:0.3.
wherein the nonionic surfactant is the compound of alkylphenol ethoxylates and fatty alcohol ethoxylates, and the mass ratio of the alkylphenol ethoxylates to the fatty alcohol ethoxylates is 1:1.
the specific amounts (in kg) of the components in examples 1 to 5 are shown in Table 2.
TABLE 2
The preparation method of the aluminum alloy acid etching solution comprises the following steps:
step 1), water is injected into a stirring kettle, sulfuric acid is added into the water, the sulfuric acid is injected at a constant speed for 10min, stirring is started while the sulfuric acid is injected, the rotating speed is 10r/min, and the stirring and cooling are continued to room temperature, so that sulfuric acid solution is obtained;
step 2), adding nitric acid into the sulfuric acid solution, injecting the nitric acid at a constant speed for 15min at a rotating speed of 10r/min, and continuously stirring and cooling to room temperature to obtain a mixed solution;
and 3) adding ammonium bifluoride and degreasing agent into the mixed solution, stirring for 10min at the rotating speed of 10r/min, and uniformly stirring to obtain the aluminum alloy acid etching solution.
Comparative example 1
The difference between the aluminum alloy acid etching solution and the example 3 is that:
the mass ratio of the ferrous sulfate, the dipropylene glycol and the nonionic surfactant is 1:1:1
Comparative example 2
The difference between the aluminum alloy acid etching solution and the example 3 is that:
the mass ratio of alkylphenol ethoxylates to fatty alcohol ethoxylates is 1:2.
comparative example 3
An aluminum alloy acid etching solution comprises the following components:
49kg of nitric acid, 15kg of sulfuric acid, 5.5kg of ammonium bifluoride, 0.5kg of degreasing agent and 30kg of water.
Wherein the degreasing agent is a compound of ferrous sulfate, dipropylene glycol and a nonionic surfactant, and the mass ratio of the ferrous sulfate to the dipropylene glycol to the nonionic surfactant is 1:0.2:0.3.
wherein the nonionic surfactant is the compound of alkylphenol ethoxylates and fatty alcohol ethoxylates, and the mass ratio of the alkylphenol ethoxylates to the fatty alcohol ethoxylates is 1:1.
the preparation method of the aluminum alloy acid etching solution comprises the following steps:
step 1), water is injected into a stirring kettle, sulfuric acid is added into the water, the sulfuric acid is injected at a constant speed for 10min, stirring is started while the sulfuric acid is injected, the rotating speed is 10r/min, and the stirring and cooling are continued to room temperature, so that sulfuric acid solution is obtained;
step 2), adding nitric acid into the sulfuric acid solution, injecting the nitric acid at a constant speed for 15min at a rotating speed of 10r/min, and continuously stirring and cooling to room temperature to obtain a mixed solution;
and 3) adding ammonium bifluoride and degreasing agent into the mixed solution, stirring for 10min at the rotating speed of 10r/min, and uniformly stirring to obtain the aluminum alloy acid etching solution.
Comparative example 4
An aluminum alloy acid etching solution comprises the following components:
15kg of nitric acid, 24.5kg of sulfuric acid, 5.5kg of ammonium bifluoride, 0.5kg of degreasing agent and 54.5kg of water.
Wherein the degreasing agent is a compound of ferrous sulfate, dipropylene glycol and a nonionic surfactant, and the mass ratio of the ferrous sulfate to the dipropylene glycol to the nonionic surfactant is 1:0.2:0.3.
wherein the nonionic surfactant is the compound of alkylphenol ethoxylates and fatty alcohol ethoxylates, and the mass ratio of the alkylphenol ethoxylates to the fatty alcohol ethoxylates is 1:1.
the preparation method of the aluminum alloy acid etching solution comprises the following steps:
step 1), water is injected into a stirring kettle, sulfuric acid is added into the water, the sulfuric acid is injected at a constant speed for 10min, stirring is started while the sulfuric acid is injected, the rotating speed is 10r/min, and the stirring and cooling are continued to room temperature, so that sulfuric acid solution is obtained;
step 2), adding nitric acid into the sulfuric acid solution, injecting the nitric acid at a constant speed for 15min at a rotating speed of 10r/min, and continuously stirring and cooling to room temperature to obtain a mixed solution;
and 3) adding ammonium bifluoride and degreasing agent into the mixed solution, stirring for 10min at the rotating speed of 10r/min, and uniformly stirring to obtain the aluminum alloy acid etching solution.
Experiment 1
The acid etching time of the aluminum alloy of each example and comparative example is detected and recorded, and the specific experimental method is as follows:
aluminum alloy 2A11 was used to make aluminum alloy sheet samples 0.1m long, 0.1m wide and 0.01m thick.
The aluminum alloy plate sample is naturally placed for 30d under the exposure environment.
Immersing the placed aluminum alloy plate in the aluminum alloy acid etching solutions of the examples and the comparative examples, and observing the immersing time required by the completely clean surface of the aluminum alloy plate, namely the aluminum alloy acid etching time.
The method for observing the soaking time required by completely cleaning the surface of the aluminum alloy plate is as follows:
six aluminum alloy plate samples are taken and respectively soaked for 1s, 5s, 15s, 30s, 1min and 5min.
Observing the surface state of each aluminum alloy plate sample after washing, for example, grease and impurities exist on the surface of a 15s plate, the surface of a 30s plate is smooth, locking acid etching time is between 15s and 30s, then taking one aluminum alloy plate sample, soaking the aluminum alloy plate sample in an aluminum alloy acid etching solution for 22s, observing after washing, if the surface of the aluminum alloy plate sample is smooth, proving that the acid etching time of the aluminum alloy plate sample is between 15s and 22s, otherwise, between 22s and 30s, and obtaining the aluminum alloy acid etching time through repeated experiments, wherein the unit is accurate to seconds.
Experiment 2
The time from acid etching to over-etching of the aluminum alloys of each example and comparative example was measured and recorded as follows:
aluminum alloy 2A11 was used to make aluminum alloy sheet samples 0.1m long, 0.1m wide and 0.01m thick.
The aluminum alloy plate sample is naturally placed for 30d under the exposure environment.
Immersing the placed aluminum alloy plate in the aluminum alloy acid etching solutions of the examples and the comparative examples, and observing the immersing time required when the brightness reduction of the surface of the aluminum alloy plate is completely started, namely the aluminum alloy acid etching time.
The method for observing the soaking time required by completely cleaning the surface of the aluminum alloy plate is as follows:
six aluminum alloy plate samples are taken and respectively soaked, and the soaking time is additionally increased by 1s, 5s, 15s, 30s, 1min and 5min on the basis of the acid etching time obtained in the experiment 1.
Observing the surface state of each aluminum alloy plate sample after washing, for example, adding a plate for additional 30s to finish, adding a plate for additional 1min to compare with the plate for additional 30s, locking the over-corrosion time to be between 30s and 1min when the brightness is reduced, then taking one aluminum alloy plate sample to soak in an aluminum alloy acid etching solution, wherein the soaking time is 45s on the basis of the acid etching time obtained in the experiment 1, taking out, immediately soaking in clear water, taking out and wiping after soaking for 5s, and observing, if the surface of the aluminum alloy plate sample is smooth, proving that the over-corrosion time of the aluminum alloy plate sample is between 45s and 1min, otherwise, adding the plate for additional 30s and 45s, and repeating the experiment for multiple times to obtain the over-corrosion time of the aluminum alloy.
The specific test data for experiments 1 and 2 are shown in Table 3.
TABLE 3 Table 3
As can be seen from the comparison of the data of example 3 and comparative example 1 in table 3, the acid etching time is prolonged when the ferrous sulfate, dipropylene glycol and nonionic surfactant are not compounded in a specific ratio, and meanwhile, the comparison of the data of examples 1, 2, 4 and 5 and comparative example 1 shows that the influence of the sulfuric acid concentration on the acid etching time is more obvious, and the selection of the degreasing agent only has an auxiliary effect.
As can be seen from the comparison of the data of example 3 and comparative example 2 in table 3, when alkylphenol ethoxylates and fatty alcohol ethoxylates were not blended in a specific ratio, the acid etching time was prolonged, and as can be seen from the comparison of the data of examples 1, 2, 4, 5 and comparative example 2, the influence of the sulfuric acid concentration on the acid etching time was more remarkable, and the specific selection of the nonionic surfactant only gave an auxiliary effect.
According to the comparison of the data of example 3 and comparative example 3 in Table 3, the influence of sulfuric acid concentration on acid etching time is larger, sulfuric acid concentration is reduced, acid etching time is obviously prolonged, efficiency is reduced, and meanwhile, over-etching time is obviously prolonged, so that the reduction of sulfuric acid concentration can be ensured to have longer buffering time, and over-etching phenomenon is effectively reduced, but example 3 also has buffering time of nearly 70 seconds, and although the buffering time is shorter than that of low-concentration sulfuric acid, about 50 seconds is enough to finish operations such as unloading, flushing and the like, thereby realizing the effects of high acid etching efficiency and difficult occurrence of over-etching phenomenon.
According to the comparison of the data of the embodiment 3 and the data of the comparative example 4 in the table 3, the reduction of the nitric acid concentration reduces the oxidizing property, the speed of generating the aluminum oxide passivation film reduces, the aluminum alloy material cannot be protected in time, the buffer time from the completion of the acid etching to the occurrence of the over-etching is shorter and only about 12 seconds, although the aluminum alloy material can be immediately taken out and soaked in clear water to remove the acid etching agent in the experiment 2, in the actual production, the aluminum alloy material is mostly large building materials, the unloading and the cleaning of the aluminum alloy material cannot be completed quickly, for example, the lifting operation is required during the unloading, the required time is relatively longer, the operations of unloading, flushing and the like are not easy to complete within about 12 seconds, the over-etching phenomenon is easy to occur, the processing quality is unstable, the material waste is increased, and the economic benefit is lower.
The present embodiment is only for explanation of the present application and is not to be construed as limiting the present application, and modifications to the present embodiment, which may not creatively contribute to the present application as required by those skilled in the art after reading the present specification, are all protected by patent laws within the scope of claims of the present application.
Claims (3)
1. An aluminum alloy acid etching solution is characterized in that: comprises the following components in parts by mass:
49-50 parts of nitric acid;
24.5-25 parts of sulfuric acid;
5.5-6 parts of ammonium bifluoride;
0.5-1 part of degreasing agent;
18-20.5 parts of water;
the total mass part is 100 parts;
the degreasing agent is a compound of ferrous sulfate, dipropylene glycol and a nonionic surfactant;
the mass ratio of the ferrous sulfate to the dipropylene glycol to the nonionic surfactant is 1:0.2:0.3;
the nonionic surfactant is a compound of alkylphenol ethoxylates and fatty alcohol ethoxylates;
the mass ratio of the alkylphenol ethoxylates to the fatty alcohol ethoxylates is 1:1.
2. a method for preparing the aluminum alloy acid etching solution according to claim 1, characterized in that: the method comprises the following steps:
step 1), water is injected into a container, sulfuric acid is added into the water, and stirring and cooling are carried out to room temperature, so as to obtain sulfuric acid solution;
step 2), adding nitric acid into the sulfuric acid solution, stirring and cooling to room temperature to obtain a mixed solution;
and 3) adding ammonium bifluoride and degreasing agent into the mixed solution, and uniformly stirring to obtain the aluminum alloy acid etching solution.
3. The method for preparing the aluminum alloy acid etching solution according to claim 2, which is characterized in that: in the step 1), sulfuric acid is injected at a constant speed and the injection time is 10min when sulfuric acid is added into water, and in the step 2), nitric acid is injected at a constant speed and the injection time is 15min when nitric acid is added into sulfuric acid solution.
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