CN113755841A - Environment-friendly fixture coating cleaning agent, preparation method and fixture cleaning method - Google Patents
Environment-friendly fixture coating cleaning agent, preparation method and fixture cleaning method Download PDFInfo
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- CN113755841A CN113755841A CN202111060702.5A CN202111060702A CN113755841A CN 113755841 A CN113755841 A CN 113755841A CN 202111060702 A CN202111060702 A CN 202111060702A CN 113755841 A CN113755841 A CN 113755841A
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- environment
- cleaning agent
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- tin
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Classifications
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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
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/30—Acidic compositions for etching other metallic material
-
- 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
- C23F1/00—Etching metallic material by chemical means
- C23F1/44—Compositions for etching metallic material from a metallic material substrate of different composition
Abstract
The invention discloses an environment-friendly fixture coating cleaning agent, a preparation method and a fixture cleaning method, and relates to the technical field of fixture coating cleaning. The cleaning agent consists of the following components in concentration: 350g/L of sulfuric acid 300-. The environment-friendly fixture plating layer cleaning agent provided by the invention is a sulfuric acid hydrogen peroxide system, and the metal tin on the fixture exists in the solution in the form of coordination substances through the complexing action of the complexing agent on the metal tin ions, and meanwhile, the hydrolysis inhibitor can avoid the hydrolysis precipitation of tin. The method has the advantages of high stripping speed, stable stripping effect, simple and convenient operation, large tin ion loading capacity, low total nitrogen, no ammonia nitrogen, no generation of a large amount of nitrogen-containing waste gas and waste water and no serious harm to the environment after multiple times of stripping.
Description
Technical Field
The invention relates to the technical field of clamp coating cleaning, in particular to an environment-friendly clamp coating cleaning agent, a preparation method and a clamp cleaning method.
Background
The Printed Circuit Board (PCB) is a carrier for electrical connection of electronic components and is manufactured by electronic printing. Solder stripping agents are often used in the production of printed circuit boards. The tin stripping agent can selectively dissolve tin on the electroplated copper layer and simultaneously prevent the copper base layer from being corroded away as much as possible. In order to make the tin stripping agent more stable, amino is usually required to be added, but a large amount of precipitates are generated along with the addition of the amino, the precipitates are easy to block a spray head, the tin stripping reaction is incomplete, the production efficiency is reduced, and even a circuit board is scrapped. Along with the development of the printed circuit board industry, the demand of the tin stripping agent which is more efficient and more environment-friendly is more and more. At present, nitric acid or fluoride is adopted on most production lines to remove a coating, but the nitric acid or the fluoride is not used by enterprises at present due to the factors of strong toxicity of the fluoride, difficult treatment of wastewater, corrosion of an insulating layer and the like. At present, enterprises use a nitric acid-ferric nitrate system, a nitric acid-alkyl sulfonic acid system and the like mostly. Wherein, the concentration of the nitric acid is generally 20-25%, and the method has the advantages of high removal rate, cleanness, thoroughness and no residue, but along with increasing importance of the country on improving the ecological environment, the method has particularly strict management on waste water and waste gas of enterprises at present. It is well known that nitric acid has a strong oxidizing property, generates a large amount of nitrogen oxides during the tin stripping process, and causes serious damage to the environment and field operators. Compared with the nitric acid system, the nitric acid sulfonic acid type tin stripping solution has higher cost. Both nitric acid systems and alkyl sulfonic acid systems generate toxic waste gas and waste water is difficult to treat.
Disclosure of Invention
The invention aims to solve the technical problem that the existing tin stripping agent of a nitric acid system or an alkyl sulfonic acid system can generate waste gas such as nitrogen-containing waste water, nitrogen oxide and the like when acting, thereby causing harm to the environment. Therefore, the invention aims to provide the environment-friendly clamp plating cleaning agent which can replace nitric acid and has no pollution to the environment, and the emission of nitrogen-containing waste water generated by using nitric acid and the harm of harmful gases such as nitrogen oxides to the environment are reduced.
The specific technical scheme provided by the invention is as follows:
the environment-friendly fixture coating cleaning agent comprises the following components in percentage by mass: 350g/L of sulfuric acid 300-.
The further technical scheme is that the hydrogen peroxide stabilizer is at least one selected from sodium benzene sulfonate, alkyl sulfonate, sodium silicate, polyacrylamide, ethylene glycol monomethyl ether, hydroxycarboxylic acid and sodium tripolyphosphate.
It should be noted that hydrogen peroxide is very easy to undergo self-hydrolysis at normal temperature, which easily results in the reduction of effective active substances in the cleaning agent and reduces the cleaning effect. Therefore, the hydrogen peroxide stabilizer is added into the cleaning agent, so that the self-hydrolysis of the hydrogen peroxide under the normal temperature condition can be greatly and effectively inhibited, and the use efficiency of the hydrogen peroxide can be effectively improved.
The tin hydrolysis inhibitor is a polyol.
The tin hydrolysis inhibitor is at least one selected from ethylene glycol, 1, 2-propylene glycol, 1-4 butanediol, 1-6 hexanediol, neopentyl glycol, glycerol, isopropanol, n-propanol, 3-hydroxyphenylglycolic acid, n-butanol, 2-butanol, cyclopentanol and cyclohexanol.
When the cleaning agent works, tin attached to the clamp can be dissolved out, and a large amount of tin can be dissolved out from the cleaning agent along with the prolonging of the service time. According to the invention, the tin hydrolysis inhibitor is added into the cleaning agent, so that the problems that a large amount of tin is hydrolyzed and separated out, precipitates block a pipeline and the difficulty and cost of subsequent treatment are increased due to continuous dissolution of tin are effectively prevented.
The further technical scheme is that the complexing agent is at least one selected from cyclohexylamine, ammonia water, ethanolamine, citric acid, tartaric acid, diethanolamide and fumaric acid.
The complexing agent used in the invention can form a compound of complex ions with metal ions in the solution, has a stable complexing constant, prevents metal tin ions from precipitating, and has a certain effect on maintaining the pH stability of the solution.
The invention also provides a preparation method of the environment-friendly fixture plating cleaning agent, which comprises the following steps:
s1, measuring a solvent with half of the total volume of the cleaning agent, gradually adding the sulfuric acid with the formula amount into the solvent, continuously stirring, and cooling to obtain a sulfuric acid solution;
and S2, sequentially adding a complexing agent, a stabilizer, a hydrolysis inhibitor and hydrogen peroxide in a formula ratio into the sulfuric acid solution obtained in the step S1, and uniformly stirring to obtain the environment-friendly clamp plating cleaning agent.
The further technical scheme is that the solvent is pure water.
The invention also provides a clamp cleaning method, which comprises the following steps:
step i: soaking the clamp to be washed in a sulfuric acid solution with the mass fraction of 5% for 10-30s, and then washing the clamp with pure water;
step ii: soaking the clamp treated in the step i in the environment-friendly clamp plating cleaning agent as defined in any one of claims 1 to 4 until the tin plating is completely removed;
step iii: and (5) washing the clamp after tin stripping, and airing for later use.
The further technical proposal is that the soaking temperature is 25-35 ℃.
The further technical scheme is that in the step ii, the soaking time is 5-10 min.
Compared with the prior art, the invention can achieve the following technical effects:
the environment-friendly fixture plating layer cleaning agent provided by the invention is a sulfuric acid hydrogen peroxide system, and the metal tin on the fixture exists in the solution in the form of coordination substances through the complexing action of the complexing agent on the metal tin ions, and meanwhile, the hydrolysis inhibitor can avoid the hydrolysis precipitation of tin.
The environment-friendly fixture coating cleaning agent provided by the invention can replace nitric acid to be used as a fixture coating cleaning agent, has the advantages of high removal speed, stable removal effect, simplicity and convenience in operation, high tin ion loading capacity, low total nitrogen and no ammonia nitrogen in solution after multiple times of deplating, and does not generate a large amount of nitrogen-containing waste gas and waste water and serious harm to the environment.
Detailed Description
The technical solutions in the examples will be clearly and completely described below. It is apparent that the embodiments to be described below are only a part of the embodiments of the present invention, and not all of them. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It will be understood that the terms "comprises" and/or "comprising," when used in this specification and the appended claims, specify the presence of stated features, integers, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and/or groups thereof.
It is also to be understood that the terminology used in the description of the embodiments of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the embodiments of the invention. As used in the description of embodiments of the present invention and the appended claims, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise.
Example 1
The embodiment of the invention provides an environment-friendly clamp plating layer cleaning agent which comprises the following components in concentration: 300g/L of sulfuric acid, 20g/L of hydrogen peroxide, 2g/L of sodium benzenesulfonate, 10g/L of cyclohexylamine and 1ppm of isopropanol, wherein the solvent is pure water.
Example 2
The embodiment of the invention provides an environment-friendly clamp plating layer cleaning agent which comprises the following components in concentration: 310g/L of sulfuric acid, 30g/L of hydrogen peroxide, 3g/L of sodium silicate, 8g/L of ethanolamine and 20ppm of ethylene glycol, and the solvent is pure water.
Example 3
The embodiment of the invention provides an environment-friendly clamp plating layer cleaning agent which comprises the following components in concentration: 320g/L of sulfuric acid, 40g/L of hydrogen peroxide, 4g/L of polyacrylamide, 6g/L of diethanolamide and 40ppm of neopentyl glycol, and the solvent is pure water.
Example 4
The embodiment of the invention provides an environment-friendly clamp plating layer cleaning agent which comprises the following components in concentration: 330g/L of sulfuric acid, 50g/L of hydrogen peroxide, 6g/L of ethylene glycol monomethyl ether, 4g/L of fumaric acid and 60ppm of glycerol, and the solvent is pure water.
Example 5
The embodiment of the invention provides an environment-friendly clamp plating layer cleaning agent which comprises the following components in concentration: 340g/L of sulfuric acid, 60g/L of hydrogen peroxide, 8g/L of sodium tripolyphosphate, 2g/L of citric acid and 80ppm of n-propanol, wherein the solvent is pure water.
Example 6
The embodiment of the invention provides an environment-friendly clamp plating layer cleaning agent which comprises the following components in concentration: 350g/L of sulfuric acid, 80g/L of hydrogen peroxide, 10g/L of hydroxycarboxylic acid, 1g/L of tartaric acid and 100ppm of cyclopentanol, and the solvent is pure water.
The invention also provides a preparation method of the environment-friendly fixture plating cleaning agent in the embodiment 1-6, which comprises the following steps:
step S1, measuring pure water with half of the total volume of the cleaning agent, gradually adding the sulfuric acid with the formula amount into the pure water, continuously stirring, and cooling to obtain a sulfuric acid solution;
and S2, sequentially adding a complexing agent, a stabilizer, a hydrolysis inhibitor and hydrogen peroxide in a formula ratio into the sulfuric acid solution obtained in the step S1, and uniformly stirring to obtain the environment-friendly clamp plating cleaning agent.
The invention also provides a method for cleaning a clamp by using the environment-friendly clamp plating cleaning agent in the embodiment 1-6, which comprises the following steps:
step i: soaking the clamp to be washed in a sulfuric acid solution with the mass fraction of 5% for 10s, activating, and then washing with pure water;
step ii: soaking the clamp treated in the step i in a deplating tank at the temperature of 30 ℃ for 10min until the tin coating is completely removed; the deplating tank is internally provided with the environment-friendly fixture plating cleaning agent.
Step iii: and (5) washing the clamp after tin stripping, and airing for later use.
Comparative example 1
The cleaning agent is nitric acid solution. The method specifically comprises the following steps: 68% concentrated nitric acid and pure water were mixed in a ratio of 1: 1 proportion to obtain nitric acid solution as the plating layer cleaning agent.
Comparative example 2
The cleaning agent consists of the following components in concentration: 350g/L of sulfuric acid, 80g/L of hydrogen peroxide, 10g/L of hydroxycarboxylic acid, 0.5g/L of tartaric acid and 100ppm of cyclopentanol, and the solvent is pure water.
Comparative example 3
The cleaning agent consists of the following components in concentration: 350g/L of sulfuric acid, 80g/L of hydrogen peroxide, 10g/L of hydroxycarboxylic acid, 100ppm of cyclopentanol and pure water as a solvent.
Verification of tin stripping effect
The experimental method comprises the following steps:
the method comprises the following steps: the tin plate was cut into rectangular plates of length L and width M, where the length and width were in cm and weighed as W before testing2(unit is g);
step two: placing the sheared tin plate in a dilute sulfuric acid solution with the mass fraction of 5% for activation, and then washing with water;
step three: clamping the tin plate by using tweezers, putting the tin plate in a tin stripping cleaning agent, and swinging for a time T (in min) until tin is completely stripped, and taking out the tin plate;
step four: washing the tin-removed plate with pure water for 5-10s, washing with 5% dilute sulfuric acid, washing with pure water, air drying or blow drying, and weighing as W1(unit is g);
step five: the tin stripping rate V is calculated according to the following formula, and the unit is mum/min,
wherein rho is the density of the tin plate and the unit is g/cm3。
The results of the tin stripping test for the cleaners of examples 1-6 and comparative examples 1-3 are shown in Table 1.
TABLE 1 results of tin stripping experiments for examples 1 to 6 and comparative examples 1 to 3
| Tin stripping rate (μm/min) | Total nitrogen (ppm) | Ammonia nitrogen (ppm) | Tin ion load (g/L) | |
| Example 1 | 5.54 | 86 | Is free of | 45 |
| Example 2 | 6.15 | 95 | Is free of | 47 |
| Example 3 | 7.23 | 97 | Is free of | 44 |
| Example 4 | 8.01 | 101 | Is free of | 49 |
| Example 5 | 8.57 | 89 | Is free of | 43 |
| Example 6 | 9.56 | 100 | Is free of | 50 |
| Comparative example 1 | 10.34 | ＞20000 | Is free of | 80 |
| Comparative example 2 | 2.14 | 97 | Is free of | 49 |
| Comparative example 3 | 1.14 | 103 | Is free of | 48 |
Note: the total nitrogen and ammonia nitrogen refer to data which are not yet deplated after the preparation of the tank.
The results in table 1 show that the environment-friendly fixture plating cleaning agent provided by the invention can replace nitric acid to be used as a fixture plating cleaning agent, has high removal speed, can completely remove a tin plating layer (the thickness of the plating layer is about 7 micrometers) within 10min, has stable removal effect, is simple and convenient to operate, has high tin ion loading capacity, and can keep low total nitrogen and no ammonia nitrogen in a solution after multiple times of deplating, does not generate a large amount of nitrogen-containing waste gas and waste water, and does not cause serious harm to the environment.
In the above embodiments, the descriptions of the respective embodiments have respective emphasis, and for parts that are not described in detail in a certain embodiment, reference may be made to related descriptions of other embodiments.
While the invention has been described with reference to specific embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (10)
1. The environment-friendly fixture coating cleaning agent is characterized by comprising the following components in concentration: 350g/L of sulfuric acid 300-.
2. The environment-friendly fixture plating cleaning agent as defined in claim 1, wherein the hydrogen peroxide stabilizer is at least one selected from sodium benzenesulfonate, alkyl sulfonate, sodium silicate, polyacrylamide, ethylene glycol monomethyl ether, hydroxycarboxylic acid, and sodium tripolyphosphate.
3. The environment-friendly fixture plating cleaning agent as defined in claim 1, wherein the tin hydrolysis inhibitor is a polyol.
4. The environment-friendly jig plating detergent as claimed in claim 3, wherein the tin hydrolysis inhibitor is at least one selected from the group consisting of ethylene glycol, 1, 2-propylene glycol, 1-4-butanediol, 1-6-hexanediol, neopentyl glycol, glycerol, isopropyl alcohol, n-propanol, 3-hydroxyphenylglycolic acid, n-butanol, 2-butanol, cyclopentanol, and cyclohexanol.
5. The environment-friendly fixture coating cleaning agent as defined in claim 1, wherein the complexing agent is at least one selected from the group consisting of cyclohexylamine, ammonia, ethanolamine, citric acid, tartaric acid, diethanolamide and fumaric acid.
6. The method for preparing the environment-friendly fixture plating cleaning agent as defined in any one of claims 1 to 5, comprising the steps of:
s1, measuring a solvent with half of the total volume of the cleaning agent, gradually adding the sulfuric acid with the formula amount into the solvent, continuously stirring, and cooling to obtain a sulfuric acid solution;
and S2, sequentially adding a complexing agent, a stabilizer, a hydrolysis inhibitor and hydrogen peroxide in a formula ratio into the sulfuric acid solution obtained in the step S1, and uniformly stirring to obtain the environment-friendly clamp plating cleaning agent.
7. The method for preparing the environment-friendly fixture plating cleaning agent as defined in claim 6, wherein the solvent is pure water.
8. A jig cleaning method is characterized by comprising the following steps:
step i: soaking the clamp to be washed in a sulfuric acid solution with the mass fraction of 5% for 10-30s, and then washing the clamp with pure water;
step ii: soaking the clamp treated in the step i in the environment-friendly clamp plating cleaning agent as defined in any one of claims 1 to 4 until the tin plating is completely removed;
step iii: and (5) washing the clamp after tin stripping, and airing for later use.
9. The jig cleaning method according to claim 8, wherein the soaking temperature in the step ii is 25 ℃ to 35 ℃.
10. The jig cleaning method according to claim 8, wherein in the step ii, the soaking time is 5 to 10 min.
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| CN202111060702.5A CN113755841A (en) | 2021-09-10 | 2021-09-10 | Environment-friendly fixture coating cleaning agent, preparation method and fixture cleaning method |
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| CN202111060702.5A CN113755841A (en) | 2021-09-10 | 2021-09-10 | Environment-friendly fixture coating cleaning agent, preparation method and fixture cleaning method |
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2021
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Application publication date: 20211207 |