CN105369267A - Connector copper alloy wire pickling solution and pickling technological method thereof - Google Patents
Connector copper alloy wire pickling solution and pickling technological method thereof Download PDFInfo
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- CN105369267A CN105369267A CN201510866158.1A CN201510866158A CN105369267A CN 105369267 A CN105369267 A CN 105369267A CN 201510866158 A CN201510866158 A CN 201510866158A CN 105369267 A CN105369267 A CN 105369267A
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- copper alloy
- alloy wire
- pickling
- pickle solution
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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
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
- C23G1/10—Other heavy metals
- C23G1/103—Other heavy metals copper or alloys of copper
Abstract
The invention discloses a connector copper alloy wire pickling solution and a pickling technological method thereof. The pickling solution and a copper alloy wire are provided. The pickling solution consists of the raw materials in parts by weight as follows: 50-90 parts of concentrated sulfuric acid, 45-70 parts of sodium nitrate and 10-20 parts of brightening agent. A preparation method of the pickling solution comprises the steps as follows: a certain amount of pure water is poured into a beaker; a certain amount of concentrated sulfuric acid is slowly poured into the beaker, and is continuously mixed with a glass rod; then weighed sodium nitrate is added, and is mixed till dissolved completely; after the temperature of a dissolved solution falls to 50-67 degrees, an appropriate amount of brightening agent soaked with cold water is added, and is mixed fully; and after the temperature of the pickling solution falls to 25-35 degrees, the pickling solution is put in a thermostatic container to be subjected to heat preservation storage. With the adoption of the pickling solution and the pickling technological method, metal losses are reduced, link pollution is reduced, and an industrial environment is improved.
Description
Technical field
The present invention relates to copper alloy wire field, be specifically related to a kind of connector copper alloy wire pickle solution and acid cleaning process method thereof.
Background technology
Copper alloy wire in the course of processing in order to eliminate material oriental cherry, need to carry out high temperature oxidation annealing, copper line surface after annealing defines and is oxidized to, copper alloy oxide skin outermost is cupric oxide, the Red copper oxide of one deck brown is also had at oxidation copper cash, in order to remove surface oxide layer, the copper cash after to annealing is needed to carry out pickling, the pickle solution formula that current most Tong Jia work enterprise uses is for running off, the solution that nitric acid and water are made into according to a certain percentage, the shortcoming of this formula is strong reaction, pickling time is slightly long just there will be copper through corrosion phenomenon, metal loss is large, a large amount of irritant gass is produced in acid cleaning process, polluted air.
Summary of the invention
For solving the problem, the invention provides a kind of connector copper alloy wire pickle solution and acid cleaning process method thereof.
For achieving the above object, the technical scheme that the present invention takes is:
A kind of connector copper alloy wire pickle solution and acid cleaning process method thereof, comprise pickle solution and copper alloy wire, described pickle solution is made up of the raw material of following weight part: the vitriol oil 50 ~ 90 parts, SODIUMNITRATE 45 ~ 70 parts, brightening agent 10 ~ 20 parts;
The configuration step of described pickle solution is as follows:
First in beaker, pour a certain amount of pure water into, more a certain amount of vitriol oil is slowly poured in beaker, and constantly stir with glass stick, then add the SODIUMNITRATE weighed up, be stirred to and dissolve completely;
Liquid temp to be dissolved is down to 50 ~ 67 DEG C, adds the brightening agent crossed through cold water soak in right amount, fully stirs;
Treat that solution temperature is down to 25 ~ 35 DEG C, put into thermostatic container insulation and deposit.
Further, comprise the steps: sample-to weigh-pickling-cold wash-saponification process-dry-weigh;
S1: take the copper alloy wire that specification is 0.88mm*4.01mm, weigh, record weight;
S2: copper alloy wire is put into ready reaction vessel, adds pickle solution and carries out pickling operation;
S3: the copper alloy wire after pickling is carried out cold water flush;
S4, the copper alloy wire after cold wash is carried out saponification process;
S5, the copper alloy wire after saponification process is carried out drying in anaerobic drying container; Weigh after oven dry, record weight.
Further, in described step S2, in pickle solution, the concentration of the vitriol oil is 260 ~ 550g/L, and the concentration of SODIUMNITRATE is 1 ~ 100g/L, and the concentration of brightening agent is 0.3 ~ 12g/L.
Further, described step S2 pickling temperature is 35 ~ 55 DEG C, and pickling time is 30 ~ 180s.
Further, the cold water in described step S3 is anaerobic pure water.
Further, in described step S5, bake out temperature is 80 ~ 90 DEG C, and the time is 5 ~ 10 minutes.
The oxide compound of the vitriol oil of the present invention and copper sends and reacts, and its concentration affects the smooth finish of copper line surface after pickling, and time vitriol oil concentration is low, hydrogen ion intensity is little, sluggish, luminance brightness is poor, when vitriol oil excessive concentration, soltion viscosity is large, and reaction is slow on the contrary, and luminance brightness is not good yet;
After SODIUMNITRATE adds, total acidity is lower than the nitric acid added, reaction is also wanted slowly, when sodium nitrate concentration is low, slowly, the Red copper oxide on copper cash top layer leaves blackspot because not cleaning up for nitrate ion and Red copper oxide speed of response, otherwise, speed of response is fast, and copper line surface easily produces excessive erosion and becomes coarse;
Brightening agent is a kind of tensio-active agent; it can Preferential adsorption in metallic surface; solid-liquid interface forms layer protecting film, and the chemical corrosion making metallic surface uneven changes regular dissolving into, and the thickness distribution on the metal surface of protective membrane is uneven.
Embodiment
In order to make objects and advantages of the present invention clearly understand, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
The present invention includes pickle solution and copper alloy wire, described pickle solution is made up of the raw material of following weight part: the vitriol oil 50 ~ 90 parts, SODIUMNITRATE 45 ~ 70 parts, brightening agent 10 ~ 20 parts;
The configuration step of described pickle solution is as follows:
First in beaker, pour a certain amount of pure water into, more a certain amount of vitriol oil is slowly poured in beaker, and constantly stir with glass stick, then add the SODIUMNITRATE weighed up, be stirred to and dissolve completely;
Liquid temp to be dissolved is down to 50 ~ 67 DEG C, adds the brightening agent crossed through cold water soak in right amount, fully stirs;
Treat that solution temperature is down to 25 ~ 35 DEG C, put into thermostatic container insulation and deposit.
A kind of connector copper alloy wire pickle solution and acid cleaning process method thereof, comprise the steps: sample-to weigh-pickling-cold wash-saponification process-dry-weigh;
S1: take the copper alloy wire that specification is 0.88mm*4.01mm, weigh, record weight;
S2: copper alloy wire is put into ready reaction vessel, adds pickle solution and carries out pickling operation, is reaction vessel is provided with nitrogen peroxide absorption unit;
S3: the copper alloy wire after pickling is carried out cold water flush;
S4, the copper alloy wire after cold wash is carried out saponification process;
S5, the copper alloy wire after saponification process is carried out drying in anaerobic drying container; Weigh after oven dry, record weight.
In described step S2, in pickle solution, the concentration of the vitriol oil is 260 ~ 550g/L, and the concentration of SODIUMNITRATE is 1 ~ 100g/L, and the concentration of brightening agent is 0.3 ~ 12g/L.
Described step S2 pickling temperature is 35 ~ 55 DEG C, and pickling time is 30 ~ 180s.
Cold water in described step S3 is anaerobic pure water.
In described step S5, bake out temperature is 80 ~ 90 DEG C, and the time is 5 ~ 10 minutes.
embodiment 1:
Take the vitriol oil 66 parts, SODIUMNITRATE 55 parts, brightening agent 15 parts;
First in beaker, pour a certain amount of pure water into, then the vitriol oil of 66 parts is slowly poured in beaker, and constantly stir with glass stick, then add the SODIUMNITRATE weighing up 55 parts, be stirred to and dissolve completely;
Liquid temp to be dissolved is down to 59 DEG C, adds the brightening agent crossed through cold water soak of 15 parts, fully stirs;
Treat that solution temperature is down to 29 DEG C, put into thermostatic container insulation and deposit.
A kind of connector copper alloy wire pickle solution and acid cleaning process method thereof, comprise the steps: sample-to weigh-pickling-cold wash-saponification process-dry-weigh;
S1: take the copper alloy wire that specification is 0.88mm*4.01mm, weigh, record weight;
S2: copper alloy wire is put into ready reaction vessel, adds pickle solution and carries out pickling operation;
S3: the copper alloy wire after pickling is carried out cold water flush;
S4, the copper alloy wire after cold wash is carried out saponification process;
S5, the copper alloy wire after saponification process is carried out drying in anaerobic drying container; Weigh after oven dry, record weight;
In described step S2, in pickle solution, the concentration of the vitriol oil is 288g/L, and the concentration of SODIUMNITRATE is 66g/L, and the concentration of brightening agent is 2g/L.
Described step S2 pickling temperature is 44 DEG C, and pickling time is 50s.
Cold water in described step S3 is anaerobic pure water.
In described step S5, bake out temperature is 88 DEG C, and the time is 6 minutes.
embodiment 2:
The vitriol oil 90 parts, SODIUMNITRATE 70 parts, brightening agent 20 parts;
The configuration step of described pickle solution is as follows:
First in beaker, pour a certain amount of pure water into, then the vitriol oil of 90 parts is slowly poured in beaker, and constantly stir with glass stick, then add the SODIUMNITRATE weighing up 70 parts, be stirred to and dissolve completely;
Liquid temp to be dissolved is down to 67 DEG C, adds the brightening agent crossed through cold water soak of 20 parts, fully stirs;
Treat that solution temperature is down to 35 DEG C, put into thermostatic container insulation and deposit.
A kind of connector copper alloy wire pickle solution and acid cleaning process method thereof, comprise the steps: sample-to weigh-pickling-cold wash-saponification process-dry-weigh;
S1: take the copper alloy wire that specification is 0.88mm*4.01mm, weigh, record weight;
S2: copper alloy wire is put into ready reaction vessel, adds pickle solution and carries out pickling operation;
S3: the copper alloy wire after pickling is carried out cold water flush;
S4, the copper alloy wire after cold wash is carried out saponification process;
S5, the copper alloy wire after saponification process is carried out drying in anaerobic drying container; Weigh after oven dry, record weight;
In described step S2, in pickle solution, the concentration of the vitriol oil is 550g/L, and the concentration of SODIUMNITRATE is 100g/L, and the concentration of brightening agent is 12g/L.
Described step S2 pickling temperature is 55 DEG C, and pickling time is 180s.
Cold water in described step S3 is anaerobic pure water.
In described step S5, bake out temperature is 89 DEG C, and the time is 9 minutes.
embodiment 3:
The vitriol oil 59 parts, SODIUMNITRATE 49 parts, brightening agent 19 parts;
The configuration step of described pickle solution is as follows:
First in beaker, pour a certain amount of pure water into, then the vitriol oil of 59 parts is slowly poured in beaker, and constantly stir with glass stick, then add the SODIUMNITRATE weighing up 49 parts, be stirred to and dissolve completely;
Liquid temp to be dissolved is down to 50 DEG C, adds the brightening agent crossed through cold water soak of 19 parts, fully stirs;
Treat that solution temperature is down to 25 DEG C, put into thermostatic container insulation and deposit.
A kind of connector copper alloy wire pickle solution and acid cleaning process method thereof, comprise the steps: sample-to weigh-pickling-cold wash-saponification process-dry-weigh;
S1: take the copper alloy wire that specification is 0.88mm*4.01mm, weigh, record weight;
S2: copper alloy wire is put into ready reaction vessel, adds pickle solution and carries out pickling operation;
S3: the copper alloy wire after pickling is carried out cold water flush;
S4, the copper alloy wire after cold wash is carried out saponification process;
S5, the copper alloy wire after saponification process is carried out drying in anaerobic drying container; Weigh after oven dry, record weight;
In described step S2, in pickle solution, the concentration of the vitriol oil is 260g/L, and the concentration of SODIUMNITRATE is 1g/L, and the concentration of brightening agent is 0.3g/L.
Described step S2 pickling temperature is 35 DEG C, and pickling time is 30s.
Cold water in described step S3 is anaerobic pure water.
In described step S5, bake out temperature is 80 DEG C, and the time is 5 minutes.
The oxide compound of the vitriol oil of the present invention and copper sends and reacts, and its concentration affects the smooth finish of copper line surface after pickling, and time vitriol oil concentration is low, hydrogen ion intensity is little, sluggish, luminance brightness is poor, when vitriol oil excessive concentration, soltion viscosity is large, and reaction is slow on the contrary, and luminance brightness is not good yet;
After SODIUMNITRATE adds, total acidity is lower than the nitric acid added, reaction is also wanted slowly, when sodium nitrate concentration is low, slowly, the Red copper oxide on copper cash top layer leaves blackspot because not cleaning up for nitrate ion and Red copper oxide speed of response, otherwise, speed of response is fast, and copper line surface easily produces excessive erosion and becomes coarse;
Brightening agent is a kind of tensio-active agent; it can Preferential adsorption in metallic surface; solid-liquid interface forms layer protecting film, and the chemical corrosion making metallic surface uneven changes regular dissolving into, and the thickness distribution on the metal surface of protective membrane is uneven.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (6)
1. a connector copper alloy wire pickle solution, is characterized in that, comprises pickle solution and copper alloy wire, and described pickle solution is made up of the raw material of following weight part: the vitriol oil 50 ~ 90 parts, SODIUMNITRATE 45 ~ 70 parts, brightening agent 10 ~ 20 parts;
The configuration step of described pickle solution is as follows:
First in beaker, pour a certain amount of pure water into, more a certain amount of vitriol oil is slowly poured in beaker, and constantly stir with glass stick, then add the SODIUMNITRATE weighed up, be stirred to and dissolve completely;
Liquid temp to be dissolved is down to 50 ~ 67 DEG C, adds the brightening agent crossed through cold water soak in right amount, fully stirs;
Treat that solution temperature is down to 25 ~ 35 DEG C, put into thermostatic container insulation and deposit.
2. connector copper alloy wire pickle solution and an acid cleaning process method thereof, is characterized in that, comprise the steps: sample-to weigh-pickling-cold wash-saponification process-dry-weigh;
S1: take the copper alloy wire that specification is 0.88mm*4.01mm, weigh, record weight;
S2: copper alloy wire is put into ready reaction vessel, adds pickle solution and carries out pickling operation;
S3: the copper alloy wire after pickling is carried out cold water flush;
S4, the copper alloy wire after cold wash is carried out saponification process;
S5, the copper alloy wire after saponification process is carried out drying in anaerobic drying container; Weigh after oven dry, record weight.
3. a kind of connector copper alloy wire pickle solution according to claim 2 and acid cleaning process method thereof, it is characterized in that, in described step S2, in pickle solution, the concentration of the vitriol oil is 260 ~ 550g/L, and the concentration of SODIUMNITRATE is 1 ~ 100g/L, and the concentration of brightening agent is 0.3 ~ 12g/L.
4. a kind of connector copper alloy wire pickle solution according to claim 2 and acid cleaning process method thereof, is characterized in that, described step S2 pickling temperature is 35 ~ 55 DEG C, and pickling time is 30 ~ 180s.
5. a kind of connector copper alloy wire pickle solution according to claim 2 and acid cleaning process method thereof, is characterized in that, the cold water in described step S3 is anaerobic pure water.
6. a kind of connector copper alloy wire pickle solution according to claim 2 and acid cleaning process method thereof, is characterized in that, in described step S5, bake out temperature is 80 ~ 90 DEG C, and the time is 5 ~ 10 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510866158.1A CN105369267A (en) | 2015-12-02 | 2015-12-02 | Connector copper alloy wire pickling solution and pickling technological method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510866158.1A CN105369267A (en) | 2015-12-02 | 2015-12-02 | Connector copper alloy wire pickling solution and pickling technological method thereof |
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| CN105369267A true CN105369267A (en) | 2016-03-02 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201510866158.1A Pending CN105369267A (en) | 2015-12-02 | 2015-12-02 | Connector copper alloy wire pickling solution and pickling technological method thereof |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1865505A (en) * | 2006-06-14 | 2006-11-22 | 内蒙古第一机械制造（集团）有限公司 | Acidwash solution for copper and copper alloy |
| JP2010222654A (en) * | 2009-03-24 | 2010-10-07 | Nippon Steel Engineering Co Ltd | Method of pickling copper-based stock |
| CN104313610A (en) * | 2014-10-10 | 2015-01-28 | 河南平高电气股份有限公司 | Environment-friendly copper and copper alloy pickling agent and copper and copper alloy silver-plating pretreatment method |
-
2015
- 2015-12-02 CN CN201510866158.1A patent/CN105369267A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1865505A (en) * | 2006-06-14 | 2006-11-22 | 内蒙古第一机械制造（集团）有限公司 | Acidwash solution for copper and copper alloy |
| JP2010222654A (en) * | 2009-03-24 | 2010-10-07 | Nippon Steel Engineering Co Ltd | Method of pickling copper-based stock |
| CN104313610A (en) * | 2014-10-10 | 2015-01-28 | 河南平高电气股份有限公司 | Environment-friendly copper and copper alloy pickling agent and copper and copper alloy silver-plating pretreatment method |
Non-Patent Citations (1)
| Title |
|---|
| 叶乘黄: ""铜及铜合金线材酸洗液配方的改进"", 《安徽化工》 * |
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Application publication date: 20160302 |