CN104099598A - Red copper chromium-free chemical conversion coating treating agent and preparation method thereof - Google Patents
Red copper chromium-free chemical conversion coating treating agent and preparation method thereof Download PDFInfo
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- CN104099598A CN104099598A CN201410357496.8A CN201410357496A CN104099598A CN 104099598 A CN104099598 A CN 104099598A CN 201410357496 A CN201410357496 A CN 201410357496A CN 104099598 A CN104099598 A CN 104099598A
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Abstract
The invention discloses a red copper chromium-free chemical conversion coating treating agent and a preparation method thereof. The treating agent comprises the following components: 8-12 g/L of a main film-forming agent, 4-8 g/L of an accelerant, 2-4 g/L of rare-earth salt, 6-10 g/L of a complexing agent, 2-4 g/L of a conditioning agent and the balance of water. Through the comparison that the red copper surface is treated by the conversion coating treating agent with that the red copper surface is treated by a chromate conversion coating treating agent through an immersion corrosion test, a zero-gravity test and a neutral salt spray test, the result shows that the corrosion resistance of the red copper surface being treated by the conversion coating treating agent is better than that of the red copper surface being treated by the chromate conversion coating treating agent, so that the chromate conversion coating treating agent can be fully replaced, and meanwhile, the red copper chromium-free chemical conversion coating treating agent provided by the invention contains no chromate, is low in price, good in corrosion resistance, convenient to use, and can be applied in practical industrial production.
Description
Technical field
The present invention relates to metal corrosion and protection technical field, be specifically related to a kind of red copper Chrome-free chemistry conversion film treating agent and preparation method thereof.
Background technology
Copper is the non-ferrous metal very close with mankind's relation, is widely used in the fields such as electric, light industry, machinofacture, building industry, national defense industry, in the consumption of China YouSe metallic substance, is only second to aluminium.Copper has good electroconductibility and processing characteristics, most widely used in electric, electronic industry, consumption is maximum, accounts for aggregate consumption over half.Wherein red copper is widely applied in industries such as cable, motor, bus, transformer, switching arrangement and the heat exchanger of electric power, pipeline, solar heat collector, electrical fittings.Therefore, copper is and the human being's production closely bound up a kind of important non-ferrous metal of living.
The Standard Electrode Potentials of copper be on the occasion of, there is good corrosion resistance nature, but running into acidity, alkaline corrosion medium or corrosion and variable color just easily occur in comparatively high temps and wet environment.In order to prevent corrosion and the variable color of copper, adopting chemical conversion film processing is the most frequently used metal protection method.The effect of conversion film is the thermodynamic stability that metallic compound that metal simple-substance active chemical property is transformed into stable chemical nature improves metal, the conversion product of metallic surface has also played certain buffer action to surrounding medium simultaneously, thereby improves the corrosion resisting property of metal.Traditional metallochemistry conversion film is processed main by chromate conversion treatments technique (also claiming chromic acid passivation), and the conversion film compact structure that the metallic surface after wherethrough reason forms, therefore has good antiseptic property to metal.But in chromic salt, contain sexavalent chrome (Cr
6+) this hypertoxic carcinogens, limited or ban use of by some countries.As European Union comes into effect the ROHS environmental protection act of Chrome-free product from July, 2006, the electric equipment products that regulation enters EU market bans use of sexavalent chrome element.Our country also puts into effect " heavy metal contamination integrated control " 12 " planning ", and the heavy metals such as mercury, chromium, cadmium, lead are carried out to emphasis prevention and control.At present, the problem of China's heavy metal environmental pollution is comparatively outstanding, has caused showing great attention to of governments at all levels, and contaminating enterprises are renovated.Therefore, exploitation asepsis environment-protecting, efficient red copper Chrome-free chemical conversion film treatment technology, extremely urgent.
Summary of the invention
The technical problem to be solved in the present invention be to provide one not good, easy to use containing chromic salt and the low solidity to corrosion of price, can be applied to industrial red copper Chrome-free chemistry conversion film treating agent,
For addressing the above problem, the present invention adopts following technical scheme:
A kind of red copper Chrome-free chemistry conversion film treating agent, comprises following material composition and content thereof:
Main membrane-forming agent 8～12g/L
Promotor 4～8g/L
Rare-earth salts 2～4g/L
Complexing agent 6～10g/L
Conditioning agent 2～4g/L
Surplus is water.
As preferred technical scheme, described main membrane-forming agent is benzotriazole, 3-amino-1, one or both of 2,4-triazole.
As preferred technical scheme, described promotor is one or both of Sodium orthomolybdate, sodium wolframate.
As preferred technical scheme, described rare-earth salts is one or both of lanthanum nitrate, cerous nitrate.
As preferred technical scheme, described complexing agent is one or both of citric acid, oxalic acid.
As preferred technical scheme, described conditioning agent is one or both of sulphosalicylic acid, Weibull.
A preparation method for red copper Chrome-free chemistry conversion film treating agent, comprises following preparation process:
1) preparation 1L red copper Chrome-free chemistry conversion film treating agent, choose main membrane-forming agent 8～12g/L, promotor 4～8g/L, rare-earth salts 2～4g/L, complexing agent 6～10g/L, conditioning agent 2～4g/L, surplus is water, after each selected component is dissolved, evenly mix, obtain treatment agent solution;
2) by the treatment agent solution obtaining in step 1), be heated to 45～50 DEG C, obtain red copper Chrome-free chemistry conversion film treating agent of the present invention.
As preferred technical scheme, the time of using obtained red copper Chrome-free chemistry conversion film treating agent to process red copper surface is 4～5min.
The invention has the beneficial effects as follows: the present invention is with benzotriazole, 3-amino-1, and 2,4-triazole is main membrane-forming agent.Benzotriazole and 3-amino-1,2,4-triazole is effective inhibiter of copper, reacts form insoluble complex compound conversion film with copper, and copper surface is played a protective role, the solidity to corrosion of conversion film is relevant with the content of main membrane-forming agent; Sodium orthomolybdate and sodium wolframate can produce synergy with main membrane-forming agent, participate in the forming process of conversion film simultaneously, thereby contribute to improve the solidity to corrosion of conversion film; Rare-earth salts has very high active and extremely strong interfacial adsorption, and in treatment agent, add appropriate rare-earth salts and can improve the bonding force of conversion film substrate, be that the conversion film of metallic surface is more fine and close, complete.Test shows, rare-earth salts content is unsuitable too high, otherwise can make the solidity to corrosion of conversion film decline; Citric acid, oxalic acid is as complexing agent, can complex copper ion, reduce copper ion concentration, and make conversion film can be evenly distributed on substrate surface, improve film quality; It is acid that sulphosalicylic acid, the Weibull aqueous solution are, and adjustable pH value can play synergy with other filmogens simultaneously.The red copper Chrome-free chemistry conversion film treating agent that the present invention obtains, the alternative sexavalent chrome (Cr that contains
6+) chromate conversion coating treatment agent, be a kind of red copper Chrome-free chemistry conversion film treating agent of nontoxic, pollution-free, environment-friendly type.Traditional chemical conversion film treatment solution, how containing poisonous carcinogens sexavalent chrome (Cr
6+), forbidden or limit by many countries, therefore research and develop new generation of environment protection Chrome-free chemistry conversion film treating agent, imperative.Through the red copper surface of conversion film treating agent processing of the present invention and the red copper surface of chromate conversion coating treatment agent processing, after immersion corrosion test, zero-G test and neutral salt spray test contrast, result shows that the solidity to corrosion of its surface conversion coating is better than the red copper surface of chromate conversion coating treatment agent processing, completely alternative traditional chromate conversion coating treatment agent.Conversion film treating agent price of the present invention is low, easy to use, can be applicable to industrial production, good market prospects.
Embodiment
Below the preferred embodiments of the present invention are described in detail, thereby so that advantages and features of the invention can be easier to be it will be appreciated by those skilled in the art that, protection scope of the present invention are made to more explicit defining.
A kind of red copper Chrome-free chemistry conversion film treating agent, comprises following material composition and content thereof:
Main membrane-forming agent 8～12g/L
Promotor 4～8g/L
Rare-earth salts 2～4g/L
Complexing agent 6～10g/L
Conditioning agent 2～4g/L
Surplus is water.
Described main membrane-forming agent is benzotriazole, 3-amino-1, one or both of 2,4-triazole.
Described promotor is one or both of Sodium orthomolybdate, sodium wolframate.
Described rare-earth salts is one or both of lanthanum nitrate, cerous nitrate.
Described complexing agent is one or both of citric acid, oxalic acid.
Described conditioning agent is one or both of sulphosalicylic acid, Weibull.
A preparation method for red copper Chrome-free chemistry conversion film treating agent, comprises following preparation process:
1) preparation 1L red copper Chrome-free chemistry conversion film treating agent, choose main membrane-forming agent 8～12g/L, promotor 4～8g/L, rare-earth salts 2～4g/L, complexing agent 6～10g/L, conditioning agent 2～4g/L, surplus is water, after each selected component is dissolved, evenly mix, obtain treatment agent solution;
2) by the treatment agent solution obtaining in step 1), be heated to 45～50 DEG C, obtain red copper Chrome-free chemistry conversion film treating agent of the present invention.
The time of processing red copper surface with obtained red copper Chrome-free chemistry conversion film treating agent is 4～5min.
The invention has the beneficial effects as follows: the present invention is with benzotriazole, 3-amino-1, and 2,4-triazole is main membrane-forming agent.Benzotriazole and 3-amino-1,2,4-triazole is effective inhibiter of copper, reacts form insoluble complex compound conversion film with copper, and copper surface is played a protective role, the solidity to corrosion of conversion film is relevant with the content of main membrane-forming agent; Sodium orthomolybdate and sodium wolframate can produce synergy with main membrane-forming agent, participate in the forming process of conversion film simultaneously, thereby contribute to improve the solidity to corrosion of conversion film; Rare-earth salts has very high active and extremely strong interfacial adsorption, and in treatment agent, add appropriate rare-earth salts and can improve the bonding force of conversion film substrate, be that the conversion film of metallic surface is more fine and close, complete.Test shows, rare-earth salts content is unsuitable too high, otherwise can make the solidity to corrosion of conversion film decline; Citric acid, oxalic acid is as complexing agent, can complex copper ion, reduce copper ion concentration, and make conversion film can be evenly distributed on substrate surface, improve film quality; It is acid that sulphosalicylic acid, the Weibull aqueous solution are, and adjustable pH value can play synergy with other filmogens simultaneously.The red copper Chrome-free chemistry conversion film treating agent that the present invention obtains, the alternative sexavalent chrome (Cr that contains
6+) chromate conversion coating treatment agent, be a kind of red copper Chrome-free chemistry conversion film treating agent of nontoxic, pollution-free, environment-friendly type.Traditional chemical conversion film treatment solution, how containing poisonous carcinogens sexavalent chrome (Cr
6+), forbidden or limit by many countries, therefore research and develop new generation of environment protection Chrome-free chemistry conversion film treating agent, imperative.Through the red copper surface of conversion film treating agent processing of the present invention and the red copper surface of chromate conversion coating treatment agent processing, after immersion corrosion test, zero-G test and neutral salt spray test contrast, result shows that the solidity to corrosion of its surface conversion coating is better than the red copper surface of chromate conversion coating treatment agent processing, completely alternative traditional chromate conversion coating treatment agent.Conversion film treating agent price of the present invention is low, easy to use, can be applicable to industrial production, good market prospects.
Embodiment 1
Preparation 1L red copper Chrome-free chemistry conversion film treating agent, for the processing of red copper surface chemical conversion film.
Get benzotriazole 6g, 3-amino-1,2,4-triazole 2g, Sodium orthomolybdate 4g, cerous nitrate 2g, citric acid 6g, Weibull 2g, surplus is water, after each selected component is dissolved, evenly mixes, and obtains treatment agent solution; By the T2 red copper of 40mm × 40mm × 1mm after ultrasonic cleaning → washing → degreasing → washing → polishing → washing → pickling → washing, put in the conversion film treating agent preparing, treatment agent temperature is 45～50 DEG C, and the treatment time is 4min, then washes, dries.Through conversion film red copper surface after treatment, rete is smooth, bright, even, the drop of resistance to nitric acid time 19.5s.
Embodiment 2
Preparation 1L red copper Chrome-free chemistry conversion film treating agent, for the processing of red copper surface chemical conversion film.
Get 3-amino-1,2,4-triazole 8g, benzotriazole 4g, Sodium orthomolybdate 2g, sodium wolframate 2g, lanthanum nitrate 3g, citric acid 4g, oxalic acid 4g, sulphosalicylic acid 3g, surplus is water, after each selected component is dissolved, evenly mix, obtain treatment agent solution; By the T2 red copper of 40mm × 40mm × 1mm after ultrasonic cleaning → washing → degreasing → washing → polishing → washing → pickling → washing, put in the conversion film treating agent preparing, treatment agent temperature is 45～50 DEG C, and the treatment time is 5min, then washes, dries.Through conversion film red copper surface after treatment, rete is smooth, bright, even, the drop of resistance to nitric acid time 20s.
Embodiment 3
Preparation 1L red copper Chrome-free chemistry conversion film treating agent, for the processing of red copper surface chemical conversion film.
Get benzotriazole 12g, Sodium orthomolybdate 6g, sodium wolframate 2g, lanthanum nitrate 2g, cerous nitrate 2g, citric acid 5g, oxalic acid 5g, sulphosalicylic acid 4g, surplus is water, after each selected component is dissolved, evenly mixes, and obtains treatment agent solution; By the T2 red copper of 40mm × 40mm × 1mm after ultrasonic cleaning → washing → degreasing → washing → polishing → washing → pickling → washing, put in the conversion film treating agent preparing, treatment agent temperature is 45～50 DEG C, and the treatment time is 5min, then washes, dries.Through conversion film red copper surface after treatment, rete is smooth, bright, even, the drop of resistance to nitric acid time 20.2s.
Embodiment 4
Preparation 1L red copper Chrome-free chemistry conversion film treating agent, for the processing of red copper surface chemical conversion film.
Get 3-amino-1,2,4-triazole 12g, Sodium orthomolybdate 7g, lanthanum nitrate 3g, oxalic acid 10g, sulphosalicylic acid 2g, Weibull 2g, surplus is water, after each selected component is dissolved, evenly mixes, and obtains treatment agent solution; By the T2 red copper of 40mm × 40mm × 1mm after ultrasonic cleaning → washing → degreasing → washing → polishing → washing → pickling → washing, put in the conversion film treating agent preparing, treatment agent temperature is 45～50 DEG C, and the treatment time is 5min, then washes, dries.Through conversion film red copper surface after treatment, rete is smooth, bright, even, the drop of resistance to nitric acid time 20.1s.
Embodiment 5
Preparation 1L red copper Chrome-free chemistry conversion film treating agent, for the processing of red copper surface chemical conversion film.
Get benzotriazole 6g, 3-amino-1,2,4-triazole 6g, Sodium orthomolybdate 8g, lanthanum nitrate 4g, citric acid 10g, sulphosalicylic acid 4g, surplus is water, after each selected component is dissolved, evenly mixes, and obtains treatment agent solution; By the T2 red copper of 40mm × 40mm × 1mm after ultrasonic cleaning → washing → degreasing → washing → polishing → washing → pickling → washing, put in the conversion film treating agent preparing, treatment agent temperature is 45～50 DEG C, and the treatment time is 5min, then washes, dries.Through conversion film red copper surface after treatment, rete is smooth, bright, even, the drop of resistance to nitric acid time 20.1s.
[0033] in above each embodiment through conversion film of the present invention sample after treatment and chromate conversion coating sample after treatment, test and neutral salt spray test gained comparing result through immersion corrosion, as shown in the table:
Table 1: various sample changes on surface in the test of 3.5wt.%NaCl solution soaking
Table 2: neutral salt spray test (NSS test) result
The above, be only the specific embodiment of the present invention, but protection scope of the present invention is not limited to this, and any variation of expecting without creative work or replacement, within all should being encompassed in protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain that claims were limited.
Claims (8)
1. a red copper Chrome-free chemistry conversion film treating agent, is characterized in that: comprise following material composition and content thereof:
Main membrane-forming agent 8～12g/L
Promotor 4～8g/L
Rare-earth salts 2～4g/L
Complexing agent 6～10g/L
Conditioning agent 2～4g/L
Surplus is water.
2. red copper Chrome-free chemistry conversion film treating agent according to claim 1, is characterized in that: described main membrane-forming agent is benzotriazole, 3-amino-1, one or both of 2,4-triazole.
3. red copper Chrome-free chemistry conversion film treating agent according to claim 1, is characterized in that: described promotor is one or both of Sodium orthomolybdate, sodium wolframate.
4. red copper Chrome-free chemistry conversion film treating agent according to claim 1, is characterized in that: described rare-earth salts is one or both of lanthanum nitrate, cerous nitrate.
5. red copper Chrome-free chemistry conversion film treating agent according to claim 1, is characterized in that: described complexing agent is one or both of citric acid, oxalic acid.
6. red copper Chrome-free chemistry conversion film treating agent according to claim 1, is characterized in that: described conditioning agent is one or both of sulphosalicylic acid, Weibull.
7. a preparation method for the chemistry of the red copper Chrome-free as described in any one in claim 1 to 6 conversion film treating agent, is characterized in that, comprises following preparation process:
Preparation 1L red copper Chrome-free chemistry conversion film treating agent, choose main membrane-forming agent 8～12g/L, promotor 4～8g/L, rare-earth salts 2～4g/L, complexing agent 6～10g/L, conditioning agent 2～4g/L, surplus is water, after each selected component is dissolved, evenly mix, obtain treatment agent solution;
By the treatment agent solution obtaining in step 1), be heated to 45～50 DEG C, obtain red copper Chrome-free chemistry conversion film treating agent of the present invention.
8. the preparation method of red copper Chrome-free chemistry conversion film treating agent according to claim 7, is characterized in that: the time of using obtained red copper Chrome-free chemistry conversion film treating agent to process red copper surface is 4～5min.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105063595A (en) * | 2015-08-18 | 2015-11-18 | 昆明理工大学 | Phytic acid passivation solution and preparing method and application thereof |
| CN106756962A (en) * | 2016-12-02 | 2017-05-31 | 机械科学研究总院青岛分院 | A kind of copper alloy surface passivation technology |
| CN106811618A (en) * | 2017-02-13 | 2017-06-09 | 东莞市佳乾新材料科技有限公司 | A kind of red copper row of environment-friendly type fastness and preparation method thereof |
| CN107058995A (en) * | 2017-04-20 | 2017-08-18 | 合肥华清金属表面处理有限责任公司 | A kind of cold-reduced sheet chrome-free tanning agent and preparation method thereof |
| WO2022110339A1 (en) * | 2020-11-27 | 2022-06-02 | 瑞声声学科技(深圳)有限公司 | Steel sheet passivation process, passivated steel sheet, and vapor chamber |
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| CN101182641A (en) * | 2007-08-02 | 2008-05-21 | 江西理工大学 | Rare-earth copper corrosion inhibitor and mat-forming treatment process thereof |
| CN101445923A (en) * | 2008-12-30 | 2009-06-03 | 罗冲 | Passivation method for brass antitarnish |
| CN102071415A (en) * | 2010-12-02 | 2011-05-25 | 合肥华清金属表面处理有限责任公司 | Rare earth modified surface treating agent for copper and copper alloys and preparation method thereof |
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Patent Citations (3)
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| CN101182641A (en) * | 2007-08-02 | 2008-05-21 | 江西理工大学 | Rare-earth copper corrosion inhibitor and mat-forming treatment process thereof |
| CN101445923A (en) * | 2008-12-30 | 2009-06-03 | 罗冲 | Passivation method for brass antitarnish |
| CN102071415A (en) * | 2010-12-02 | 2011-05-25 | 合肥华清金属表面处理有限责任公司 | Rare earth modified surface treating agent for copper and copper alloys and preparation method thereof |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105063595A (en) * | 2015-08-18 | 2015-11-18 | 昆明理工大学 | Phytic acid passivation solution and preparing method and application thereof |
| CN106756962A (en) * | 2016-12-02 | 2017-05-31 | 机械科学研究总院青岛分院 | A kind of copper alloy surface passivation technology |
| CN106811618A (en) * | 2017-02-13 | 2017-06-09 | 东莞市佳乾新材料科技有限公司 | A kind of red copper row of environment-friendly type fastness and preparation method thereof |
| CN107058995A (en) * | 2017-04-20 | 2017-08-18 | 合肥华清金属表面处理有限责任公司 | A kind of cold-reduced sheet chrome-free tanning agent and preparation method thereof |
| CN107058995B (en) * | 2017-04-20 | 2019-01-04 | 合肥华清金属表面处理有限责任公司 | A kind of cold-reduced sheet chrome-free tanning agent and preparation method thereof |
| WO2022110339A1 (en) * | 2020-11-27 | 2022-06-02 | 瑞声声学科技(深圳)有限公司 | Steel sheet passivation process, passivated steel sheet, and vapor chamber |
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Application publication date: 20141015 |