Aluminum alloy surface chemical polishing additive and preparation method thereof
Through the introduction of the ingredients and twins to the aluminized throwing additives to the surface of the aluminum alloy surface, the problem of uneven polishing surface in the existing technologies in the existing technology is solved, and the high brightness and anti -corrosion effect of the aluminum alloy surface are achieved.
Patent Information
- Application Number
- CN202411493779.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-24
- Publication Date
- 2025-01-24
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Figure BDA0005100748860000071 
Figure BDA0005100748860000081
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of metal surface treatment, and in particular to an aluminum alloy surface polishing additive and a preparation method thereof. Background Art
[0002] Aluminum is one of the most important non-ferrous metal materials and is widely used in many fields. In order to meet different application requirements, aluminum products are required to have different surface effects, such as soft sand surface or bright mirror surface. Polishing is an important means to obtain a bright mirror surface. Although mechanical polishing can obtain a smooth and clean surface, the surface of the aluminum product is subjected to pressure and local high temperature operation during the mechanical polishing process, resulting in lattice deformation. If anodizing is performed directly without chemical polishing, an oxide film layer with a high reflective coefficient cannot be obtained, and it is difficult to obtain an ideal brightness. Therefore, after mechanical polishing, chemical polishing or electrochemical polishing must be performed to remove the surface crystal deformation layer in order to obtain a high-quality film layer with good surface decoration.
[0003] Chemical polishing of aluminum alloys usually adopts a three-acid process containing phosphoric acid, sulfuric acid and nitric acid. However, due to the strong oxidizing property of nitric acid and the characteristics of nitric acid itself, as well as the fluctuation of acid concentration, the brightness of the polished surface will be uneven. Therefore, the current chemical polishing additives for aluminum alloys basically use phosphoric acid-based chemicals supplemented with other additives. Summary of the invention
[0004] In order to solve the above technical problems, the present invention provides an aluminum alloy surface polishing additive and a preparation method thereof.
[0005] The purpose of the present invention can be achieved through the following technical solutions:
[0006] An aluminum alloy surface polishing additive comprises the following raw materials in parts by weight: 60-80 parts of phosphoric acid, 5-15 parts of sulfuric acid, 2-5 parts of corrosion inhibitor, 1-2 parts of complexing agent, 10-15 parts of brightener, and 500-600 parts of water;
[0007] The corrosion inhibitor is prepared by the following steps:
[0008] Step S1, adding L-lysine and potassium hydroxide into a glass mortar, grinding at a speed of 150r / min for 2min, then adding salicylaldehyde, and continuing grinding for 5min. After grinding, transferring to a watch glass, placing in a vacuum drying oven for 4h, to obtain intermediate 1, wherein the amount ratio of L-lysine, potassium hydroxide and salicylaldehyde is controlled to be 10-15mmol:10-15mmol:10-15mmol;
[0009] In step S1, intermediate 1 is prepared by reacting L-lysine with salicylaldehyde. The intermediate 1 has a Schiff base structure, which contains a C=N bond and electronegative atoms such as N and O. It has good coordination ability and can form a complex with transition metals. It is adsorbed on the surface of metal materials and forms a tight hydrophobic molecular film to prevent the corrosion of the metal by the corrosive medium.
[0010] Step S2, adding intermediate 1 to a 10% hydrochloric acid solution, stirring at a uniform speed and slowly dropping cyclopentanone, then heating to 80°C, stirring at a uniform speed and reacting for 4 hours, and obtaining intermediate 2 after the reaction is completed, wherein the amount ratio of intermediate 1, cyclopentanone and hydrochloric acid solution is controlled to be 5-10 mmol: 5-10 mmol: 20 mL;
[0011] In step S2, the amino group on the intermediate 1 reacts with cyclopentanone to obtain the intermediate 2, which has a quinoline structure;
[0012] Step S3, adding the prepared intermediate 2 to anhydrous ethanol, stirring at a uniform speed and slowly adding 1,8-dibromooctane, heating to reflux after the addition is completed, and reflux reaction is carried out for 48 hours. After the reaction is completed, a corrosion inhibitor is obtained, and the amount ratio of the intermediate 2, 1,8-dibromooctane and anhydrous ethanol is controlled to be 4-8mmo:8-15mmo l:30mL.
[0013] In step S3, the quinoline structure on the intermediate 2 undergoes a quaternization reaction with 1,8-dibromooctane to obtain a corrosion inhibitor. The corrosion inhibitor has a Schiff base structure on the one hand and a gemini quaternary ammonium salt structure on the other hand. The gemini quaternary ammonium salt structure can cooperate with the Schiff base structure to bring an excellent sustained-release effect to the corrosion inhibitor, thereby preventing the aluminum alloy surface from being corroded.
[0014] Furthermore, the complexing agent is a mixture of one or more of sodium gluconate, sodium alginate, ethanolamine and EDTA in any proportion.
[0015] Furthermore, the brightener is a mixture of one or more of ferrous sulfate, ferrous sulfate, copper sulfate and zinc sulfate in any proportion.
[0016] A method for preparing an aluminum alloy surface polishing additive comprises the following steps:
[0017] Add phosphoric acid, sulfuric acid, corrosion inhibitor, complexing agent, brightener and water into the reaction kettle in sequence, heat to 30-40°C, stir at a constant speed for 3-5h, and prepare the aluminum alloy surface polishing additive.
[0018] Beneficial effects of the present invention:
[0019] The invention prepares an aluminum alloy surface polishing additive, uses phosphoric acid and phosphoric acid as two-acid processes for chemical polishing, and introduces a corrosion inhibitor to prevent the aluminum alloy surface from being corroded by acid. In the preparation process of the corrosion inhibitor, L-lysine and salicylaldehyde are first reacted to prepare an intermediate 1, and the intermediate 1 has a Schiff base structure. The Schiff base structure contains a C=N bond and electronegative atoms such as N and O, has good coordination ability, can form a complex with a transition metal, is adsorbed on the surface of a metal material and forms a tight hydrophobic molecular film to block corrosion of the metal by a corrosive medium. Then, the amino group on the intermediate 1 reacts with cyclopentanone to obtain an intermediate 2, and the intermediate 2 has a quinoline structure. The quinoline structure reacts with 1,8-dibromooctane to undergo a quaternization reaction to obtain the corrosion inhibitor. The corrosion inhibitor has a Schiff base structure on one hand and a gemini quaternary ammonium salt structure on the other hand. The gemini quaternary ammonium salt structure can cooperate with the Schiff base structure to bring an excellent slow-release effect to the corrosion inhibitor, so as to prevent the aluminum alloy surface from being corroded. DETAILED DESCRIPTION
[0020] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0021] Example 1
[0022] An aluminum alloy surface polishing additive comprises the following raw materials in parts by weight: 60 parts of phosphoric acid, 5 parts of sulfuric acid, 2 parts of corrosion inhibitor, 1 part of complexing agent, 10 parts of brightener, and 500 parts of water;
[0023] A method for preparing an aluminum alloy surface polishing additive comprises the following steps:
[0024] Phosphoric acid, sulfuric acid, corrosion inhibitor, complexing agent, brightener and water were added into the reaction kettle in sequence, the temperature was raised to 30°C, and the mixture was stirred at a constant speed for 3 hours to obtain an aluminum alloy surface polishing additive.
[0025] The corrosion inhibitor is prepared by the following steps:
[0026] Step S1, adding L-lysine and potassium hydroxide into a glass mortar, grinding at a speed of 150 r / min for 2 min, then adding salicylaldehyde, and continuing grinding for 5 min. After grinding, transferring to a watch glass, placing in a vacuum drying oven for 4 h, to obtain intermediate 1, wherein the amount ratio of L-lysine, potassium hydroxide and salicylaldehyde is controlled to be 10 mmol: 10 mmol: 10 mmol;
[0027] Step S2, adding intermediate 1 to a 10% hydrochloric acid solution, stirring at a uniform speed and slowly dropping cyclopentanone, then heating to 80°C, stirring at a uniform speed and reacting for 4 hours, and obtaining intermediate 2 after the reaction is completed, wherein the amount ratio of intermediate 1, cyclopentanone and hydrochloric acid solution is controlled to be 5 mmol: 5 mmol: 20 mL;
[0028] Step S3, adding the prepared intermediate 2 to anhydrous ethanol, stirring at a uniform speed and slowly adding 1,8-dibromooctane, heating to reflux after the addition is completed, and reflux reaction is carried out for 48 hours. After the reaction is completed, a corrosion inhibitor is obtained, and the amount ratio of the intermediate 2, 1,8-dibromooctane and anhydrous ethanol is controlled to be 4mmo:8mmo l:30mL.
[0029] The complexing agent is sodium gluconate.
[0030] The brightener is ferric sulfate.
[0031] Example 2
[0032] An aluminum alloy surface polishing additive, comprising the following raw materials by weight: 65 parts of phosphoric acid, 10 parts of sulfuric acid, 3 parts of corrosion inhibitor, 1.5 parts of complexing agent, 12 parts of brightener, and 550 parts of water;
[0033] A method for preparing an aluminum alloy surface polishing additive comprises the following steps:
[0034] Phosphoric acid, sulfuric acid, corrosion inhibitor, complexing agent, brightener and water were added into the reaction kettle in sequence, the temperature was raised to 35°C, and the mixture was stirred at a constant speed for 4 hours to obtain an aluminum alloy surface polishing additive.
[0035] The corrosion inhibitor is prepared by the following steps:
[0036] Step S1, adding L-lysine and potassium hydroxide into a glass mortar, grinding at a speed of 150 r / min for 2 min, then adding salicylaldehyde, and continuing grinding for 5 min. After grinding, transferring to a watch glass, placing in a vacuum drying oven for 4 h, to obtain intermediate 1, wherein the amount ratio of L-lysine, potassium hydroxide and salicylaldehyde is controlled to be 12 mmol: 12 mmol: 12 mmol;
[0037] Step S2, adding intermediate 1 to a 10% hydrochloric acid solution, stirring at a uniform speed and slowly dropping cyclopentanone, then heating to 80°C, stirring at a uniform speed and reacting for 4 hours, and obtaining intermediate 2 after the reaction is completed, wherein the amount ratio of intermediate 1, cyclopentanone and hydrochloric acid solution is controlled to be 6 mmol: 6 mmol: 20 mL;
[0038] Step S3, adding the prepared intermediate 2 to anhydrous ethanol, stirring at a uniform speed and slowly adding 1,8-dibromooctane, heating to reflux after the addition is completed, and reflux reaction is carried out for 48 hours. After the reaction is completed, a corrosion inhibitor is obtained, and the amount ratio of the intermediate 2, 1,8-dibromooctane and anhydrous ethanol is controlled to be 6mmo:10mmo l:30mL.
[0039] The complexing agent is sodium alginate.
[0040] The brightener is ferrous sulfate.
[0041] Example 3
[0042] An aluminum alloy surface polishing additive, comprising the following raw materials by weight: 70 parts of phosphoric acid, 12 parts of sulfuric acid, 4 parts of corrosion inhibitor, 1.5 parts of complexing agent, 14 parts of brightener, and 580 parts of water;
[0043] A method for preparing an aluminum alloy surface polishing additive comprises the following steps:
[0044] Phosphoric acid, sulfuric acid, corrosion inhibitor, complexing agent, brightener and water were added into the reaction kettle in sequence, the temperature was raised to 40°C, and the mixture was stirred at a constant speed for 5 hours to obtain an aluminum alloy surface polishing additive.
[0045] The corrosion inhibitor is prepared by the following steps:
[0046] Step S1, adding L-lysine and potassium hydroxide into a glass mortar, grinding at a speed of 150 r / min for 2 min, then adding salicylaldehyde, and continuing grinding for 5 min. After grinding, transferring to a watch glass, placing in a vacuum drying oven for 4 h, to obtain intermediate 1, wherein the amount ratio of L-lysine, potassium hydroxide and salicylaldehyde is controlled to be 14 mmol: 14 mmol: 14 mmol;
[0047] Step S2, adding intermediate 1 to a 10% hydrochloric acid solution, stirring at a uniform speed and slowly dropping cyclopentanone, then heating to 80°C, stirring at a uniform speed and reacting for 4 hours, and obtaining intermediate 2 after the reaction is completed, wherein the amount ratio of intermediate 1, cyclopentanone and hydrochloric acid solution is controlled to be 8 mmol: 8 mmol: 20 mL;
[0048] Step S3, adding the prepared intermediate 2 to anhydrous ethanol, stirring at a uniform speed and slowly adding 1,8-dibromooctane, heating to reflux after the addition is completed, and reflux reaction is carried out for 48 hours. After the reaction is completed, a corrosion inhibitor is obtained, and the amount ratio of the intermediate 2, 1,8-dibromooctane and anhydrous ethanol is controlled to be 6mmo:12mmo l:30mL.
[0049] The complexing agent is ethanolamine.
[0050] The brightener is copper sulfate.
[0051] Example 4
[0052] An aluminum alloy surface polishing additive comprises the following raw materials in parts by weight: 80 parts of phosphoric acid, 15 parts of sulfuric acid, 5 parts of corrosion inhibitor, 2 parts of complexing agent, 15 parts of brightener, and 600 parts of water;
[0053] A method for preparing an aluminum alloy surface polishing additive comprises the following steps:
[0054] Phosphoric acid, sulfuric acid, corrosion inhibitor, complexing agent, brightener and water were added into the reaction kettle in sequence, the temperature was raised to 40°C, and the mixture was stirred at a constant speed for 5 hours to obtain an aluminum alloy surface polishing additive.
[0055] The corrosion inhibitor is prepared by the following steps:
[0056] Step S1, adding L-lysine and potassium hydroxide into a glass mortar, grinding at a speed of 150 r / min for 2 min, then adding salicylaldehyde, and continuing grinding for 5 min. After grinding, transferring to a watch glass, placing in a vacuum drying oven for 4 h, to obtain intermediate 1, wherein the amount ratio of L-lysine, potassium hydroxide and salicylaldehyde is controlled to be 15 mmol: 15 mmol: 15 mmol;
[0057] Step S2, adding intermediate 1 to a 10% hydrochloric acid solution, stirring at a uniform speed and slowly dropping cyclopentanone, then heating to 80°C, stirring at a uniform speed and reacting for 4 hours, and obtaining intermediate 2 after the reaction is completed, wherein the amount ratio of intermediate 1, cyclopentanone and hydrochloric acid solution is controlled to be 10 mmol: 10 mmol: 20 mL;
[0058] Step S3, adding the prepared intermediate 2 to anhydrous ethanol, stirring at a uniform speed and slowly adding 1,8-dibromooctane, heating to reflux after the addition is completed, and reflux reaction is carried out for 48 hours. After the reaction is completed, a corrosion inhibitor is obtained, and the amount ratio of the intermediate 2, 1,8-dibromooctane and anhydrous ethanol is controlled to be 8mmo:15mmol:30mL.
[0059] The complexing agent is EDTA.
[0060] The brightener is zinc sulfate.
[0061] Comparative Example 1
[0062] Compared with Example 4, this comparative example uses Intermediate 1 as a corrosion inhibitor, and the rest is the same as Example 4. The preparation method of the aluminum alloy surface polishing additive comprises the following steps:
[0063] Phosphoric acid, sulfuric acid, the intermediate 1 prepared in Example 4, a complexing agent, a brightener and water were added to a reaction kettle in sequence, the temperature was raised to 40° C., and the mixture was stirred at a constant speed for 5 hours to obtain an aluminum alloy surface polishing additive.
[0064] Comparative Example 2
[0065] The comparative example is a chemical polishing agent produced by a certain company on the market.
[0066] The performance of the aluminum alloy surface polishing additives prepared in Examples 1-4 and Comparative Examples 1-3 was tested, and the results are shown in Table 1 below:
[0067] Polishing conditions: polishing temperature is 75°C, polishing time is 60s, and polishing effect is shown in Table 1 below (wherein the 60° glossiness is obtained by calculating the average value after sampling on the sample according to the five-point sampling method).
[0068] Table 1
[0069]
[0070]
[0071] It can be seen from Table 1 above that the polishing additives prepared in Examples 1-4 of the present invention not only have excellent polishing effects, but also can protect the surface of the aluminum alloy and prevent damage to the surface of the aluminum alloy.
[0072] The above contents are merely examples and explanations of the concept of the present invention. The technicians in this technical field may make various modifications or additions to the specific embodiments described or replace them in a similar manner. As long as they do not deviate from the concept of the invention or exceed the scope defined by the claims, they should all fall within the protection scope of the present invention.
Claims
1. An aluminum alloy surface polishing additive, characterized in that: The invention comprises the following raw materials in parts by weight: 60-80 parts of phosphoric acid, 5-15 parts of sulfuric acid, 2-5 parts of corrosion inhibitor, 1-2 parts of complexing agent, 10-15 parts of brightener, and 500-600 parts of water; The corrosion inhibitor is prepared by the following steps: Step S1, adding L-lysine and potassium hydroxide into a glass mortar, grinding at a speed of 150 r / min for 2 min, then adding salicylaldehyde, and continuing grinding for 5 min. After grinding, transferring to a watch glass, placing in a vacuum drying oven and drying for 4 h, to obtain intermediate 1; Step S2, adding intermediate 1 to a 10% by mass hydrochloric acid solution, stirring at a uniform speed and slowly adding cyclopentanone dropwise, then heating to 80° C., stirring at a uniform speed and reacting for 4 hours, and obtaining intermediate 2 after the reaction is completed; Step S3, adding the prepared intermediate 2 to anhydrous ethanol, stirring at a uniform speed and slowly adding 1,8-dibromooctane, raising the temperature to reflux after the dropwise addition is completed, and reflux reaction is carried out for 48 hours. After the reaction is completed, a corrosion inhibitor is obtained.
2. The aluminum alloy surface polishing additive according to claim 1, characterized in that: In step S1, the dosage ratio of L-lysine, potassium hydroxide and salicylaldehyde is controlled to be 10-15 mmol: 10-15 mmol: 10-15 mmol.
3. The aluminum alloy surface polishing additive according to claim 1, characterized in that: In step S2, the dosage ratio of intermediate 1, cyclopentanone and hydrochloric acid solution is controlled to be 5-10 mmol: 5-10 mmol: 20 mL.
4. The aluminum alloy surface polishing additive according to claim 1, characterized in that: In step S3, the dosage ratio of the intermediate 2, 1,8-dibromooctane and anhydrous ethanol is controlled to be 4-8 mmol: 8-15 mmol: 30 mL.
5. The aluminum alloy surface polishing additive according to claim 1, characterized in that: The complexing agent is a mixture of one or more of sodium gluconate, sodium alginate, ethanolamine and EDTA in any proportion.
6. The aluminum alloy surface polishing additive according to claim 1, characterized in that: The brightener is a mixture of one or more of ferrous sulfate, ferrous sulfate, copper sulfate and zinc sulfate in any proportion.
7. The method for preparing an aluminum alloy surface polishing additive according to claim 1, characterized in that: The steps include: Add phosphoric acid, sulfuric acid, corrosion inhibitor, complexing agent, brightener and water into the reaction kettle in sequence, heat to 30-40°C, stir at a constant speed for 3-5h, and prepare the aluminum alloy surface polishing additive.