CN101139715A - Metal scavenger composition and method for producing the same - Google Patents
Metal scavenger composition and method for producing the same Download PDFInfo
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- CN101139715A CN101139715A CNA2007100309068A CN200710030906A CN101139715A CN 101139715 A CN101139715 A CN 101139715A CN A2007100309068 A CNA2007100309068 A CN A2007100309068A CN 200710030906 A CN200710030906 A CN 200710030906A CN 101139715 A CN101139715 A CN 101139715A
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- metal scavenger
- scavenger composition
- benzotriazole
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Abstract
The invention discloses a metal-removing agent combination for removing pure tin, tin-lead or tin-copper alloy on printed circuit boards and a production method for the metal-removing agent combination, which comprises components based on the weight percentage that: iron nitrate of 15.9 to 16.3 per cent, urea of 0.3 to 0.4 per cent, benzotriazole of 0.3 to 0.4 per cent, methyl benzotriazole; 0.2 to 0.3 per cent, hydrochloric acid of 1.5 to 1.7 per cent, nitric acid of 33 to 36 per cent, and the remainder water. The method for producing the removing agent combination comprises the procedures of: (1) adding in sequence according to proportion the raw materials nitric acid, iron nitrate, hydrochloric acid, urea, benzotriazole, methyl benzotriazole and water in a production tank; (2) agitating till the raw materials solve completely, and inspecting. The metal-removing agent combination is a standalone fluid, can erode rapidly any foreign matters on a copper surface while maintaining a very low eroding rate to the copper, comprises no fluoride and will not erode the base material, has high removing speed, low environmental pollution, and wide applicability and operation convenience.
Description
Technical field
The present invention relates to a kind of chemical metal scavenger, more definitely relate to a kind of metal scavenger composition and production method thereof that pure tin, tin lead or gun-metal that substrate surface forms are removed in the printed-wiring board (PWB) Production Flow Chart that be applied to.
Background technology
General printed-wiring board (PWB) has the copper conductor figure on insulating base, usually by electroplating tin or solder coating on described copper base, generate tin or tinsel film coating.At present, after producing the etching of PCB negative film flow process, need to remove tin, tin lead or the impurity such as gun-metal and scolder of copper face, industry is general employed scavenging agent solution in the past, the general composition that uses two types, the most widely used composition was based on the acidic solution that comprises peroxidation fluorine and fluorochemical in the past.In recent years, the industrial ingredients that is extensive use of based on the salpeter solution that comprises iron ion that changes into.
Use superoxide-fluoride aqueous solution when removing thermopositive reaction can take place, make solution be heated to the temperature that can make unsettled peroxide breakdown, thereby solution can not be used, therefore, this solution needs cooling in use.And the effect of superoxide-fluoride aqueous solution is slower than salpeter solution.
Salpeter solution has been eliminated the problem of superoxide-fluoride aqueous solution.Early stage salpeter solution is used in combination based on many liquid, first acidic solution comprises nitric acid removing tin or scolder, and second acidic solution comprises the mixture of iron(ic) chloride, ammonium persulphate, sulfuric acid and hydrogen peroxide or tart superoxide-fluorochemical mixture with dissolving tin lead or gun-metal.In the recent period, also mixed thionamic acid or halogen ion on the basis of above-mentioned acidic solution, its effect helps to suppress the erosion of copper and removes other alloy and pollutent.
Its tin of the said products, tin lead and tin copper corrosion amount are all lower, in use corrode ground and copper face easily, make copper face produce oxidation, reduce insulation resistance, influence the quality of printed-wiring board (PWB), use inconvenience simultaneously, stripping tin speed is slower, it is not high that the waste liquid that produces is difficult for handling recovery value, easily causes environmental pollution.
Summary of the invention
The objective of the invention is for overcoming the shortcoming of the said products, a kind of have high corrosion tin, tin lead and gun-metal amount are provided, extremely low to erosion copper speed simultaneously, the metal scavenger composition of the suitability and the operation ease of broad is arranged.
Metal scavenger composition of the present invention, composed of the following components by weight percentage:
Iron nitrate 15.9%～16.3%
Urea 0.3%～0.4%
Benzotriazole 0.3%～0.4%
Tolyltriazole 0.2%～0.3%
Hydrochloric acid 1.5%～1.7%
Nitric acid 33%～36%
Residue is water.
In above-mentioned metal scavenger composition, the content of iron nitrate is preferably 16.1%, content of urea is preferably 0.4%, the content of benzotriazole is preferably 0.4%, the content of tolyltriazole is preferably 0.3%, the content of hydrochloric acid is preferably 1.6%, and the content of nitric acid is preferably 35%, and the content of water is preferably 46.2%.
Used wet concentration tap water, distilled water, deionized water or softening water naturally in the metal scavenger composition of the present invention, wherein tap water most preferably.
Another object of the present invention provides a kind of method of producing above-mentioned metal scavenger composition, and this production method may further comprise the steps:
At normal temperatures and pressures
1. in producing groove, proportionally add starting material nitric acid, iron nitrate, hydrochloric acid, urea, benzotriazole, tolyltriazole and water successively;
2. test after the dissolving through being stirred to fully.
Each component in the above-mentioned metal scavenger composition all can be buied from the market, by those skilled in the art is understood.
The principal reaction formula of described metal scavenger composition in it is used is:
HNO3+Sn→SnNO
3+H
2O
The principal reaction step of described metal scavenger composition in it is used is:
Tin Huo Tin lead → oxidation → Yangization Tin/plumbous oxide → dissolving → soluble compound
Copper Tin alloy → oxidation → soluble compound
Copper Tin alloy → oxidation → soluble compound
In described metal scavenger composition; nitric acid is the major function composition; in reaction, play the dissolution of metals effect; iron nitrate, hydrochloric acid and urea can make speed of response accelerate in reaction; and benzotriazole can protect copper face anti-oxidant in reaction, and tolyltriazole is in order to prevent that precipitation from producing in reaction.
The effect in removing copper face impurity of the known nitric acid of those skilled in the art, iron nitrate, but and do not know the combined action of nitric acid, iron nitrate, hydrochloric acid, urea, benzotriazole and tolyltriazole in single prescription.
Metal scavenger composition of the present invention is realized can keeping extremely hanging down of copper lost speed in the high corrosion copper face impurity in application, does not contain any fluorochemical, thus do not corrode ground, and removing speed is fast, and environmental pollution is little.
Embodiment
One. the composition of described metal scavenger composition:
Be iron nitrate 15.9%～16.3%, urea 0.3%～0.4%, benzotriazole 0.3%～0.4%, tolyltriazole 0.2%～0.3%, hydrochloric acid 1.5%～1.7%, nitric acid 33%～36% by weight percentage, remain and be water.The water of component is a kind of in tap water, distilled water, deionized water or the softening water, wherein tap water most preferably.
Two. the embodiment of described metal scavenger composition:
To make 100 kilograms of amounts is example:
Embodiment 1
15.9 kilograms of iron nitrates, 0.3 kilogram in urea, 0.3 kilogram of benzotriazole, 0.2 kilogram of tolyltriazole, 1.5 kilograms of hydrochloric acid, 33 kilograms in nitric acid, 48.8 kilograms in water.
Embodiment 2
16.1 kilograms of iron nitrates, 0.4 kilogram in urea, 0.4 kilogram of benzotriazole, 0.3 kilogram of tolyltriazole, 1.6 kilograms of hydrochloric acid, 35 kilograms in nitric acid, 46.2 kilograms in water.
Embodiment 3
16.3 kilograms of iron nitrates, 0.4 kilogram in urea, 0.4 kilogram of benzotriazole, 0.3 kilogram of tolyltriazole, 1.7 kilograms of hydrochloric acid, 36 kilograms in nitric acid, 44.9 kilograms in water.
Three. the making method of described metal scavenger composition:
At normal temperatures and pressures
1. in producing groove, proportionally add starting material nitric acid, iron nitrate, hydrochloric acid, urea, benzotriazole, tolyltriazole and water successively;
2. test after the dissolving through being stirred to fully.
Four. the product specification of described metal scavenger composition:
Outward appearance: yellow pourable liquid
Proportion (25 ℃): 1.26+/-0.02
Acid equivalent:＞6.5N
Five. the operating method of described metal scavenger composition on producing:
Spray pattern, and can take discharging to add or add automatically.
Join groove: open cylinder liquid stoste and directly join groove, service temperature is controlled between 25-40 ℃;
Add:
A. discharging is added:
Increase along with doing the plate amount, acidity reduces, and moves back tin speed and slows down gradually, and when speed is reduced to a certain value, and still moves back tin when clean, can add an amount of annex solution, adds its tank liquor acid number of back and is controlled between the 4.5-5.5N.
B. add automatically:
Adorn a specific gravity control device, when tank liquor proportion is higher than a certain value, promptly start add-on system, the metal scavenger annex solution is added in the groove, when tank liquor proportion was reduced to a certain value, system promptly stopped interpolation automatically, greatly handled easily and enhancing productivity.
Six. the tin that moves back of described metal scavenger composition is tested:
Experiment condition:
(1) acid number is 5.4N, sampling 150ml.
(2) tin sheet (having placed a wheat harvesting period) is of a size of 5.5cm*3.5cm.
(3) room temperature is 30 ℃, without water coolant, and swing tin sheet when moving back tin.
Experimental result is as follows:
| The sheet number | Move back the tin time (S) | Temperature (℃) |
| 1 | 55 | 30 |
| 2 | 55 | 31 |
| 3 | 60 | 32 |
| 4 | 60 | 33 |
| 5 | 55 | 34 |
| 6 | 60 | 35 |
| 7 | 55 | 36 |
| 8 | 65 | 36.5 |
| 9 | 70 | 37 |
| 10 | 70 | 37.5 |
| 11 | 70 | 38 |
| 12 | 70 | 38.5 |
| 13 | 70 | 39 |
| 14 | 70 | 39.3 |
| 15 | 75 | 39.7 |
| 16 | 75 | 40 |
| 17 | 40 |
By above experimental data as can be known, described scavenging agent heats up in moving back the tin process slowly.
Seven. the analytical procedure of described metal scavenger composition:
1. the mensuration of acid equivalent:
Required reagent: 0.1N NaOH, methyl red indicator
Step: a. gets the 5ml tank liquor in the 100ml measuring bottle, adds pure water to scale.
B. get the 5ml diluent in 250ml taper measuring bottle, add DI water 50ml.
C. add 5 methyl red indicators.
D. use 0.1N NaOH titration, it is terminal point that color becomes yellow by redness.
Calculate: acid equivalent=N.V (ml) .4
By actual production, tin or tin lead at described metal scavenger liquid medicine plate face when acid number is 4.0N can divest totally fully, but the unclean phenomenon of tin might appear shelling in indivedual planks when acid number was lower than 4.0N, so chemical concentration is controlled at more than the acid number 4.0N and can guarantees good quality when actual production, owing to contain special antioxidant (benzotriazole) in the product, so copper face is difficult for oxidation, by to the actual measurement in producing, erosion copper amount is 12 μ " below/min; contain about 100～150g/L tin in the reacted wastewater, the acid about 4N.
Claims (12)
1. metal scavenger composition is characterized in that said composition is composed of the following components by weight percentage:
Iron nitrate 15.9%～16.3%
Urea 0.3%～0.4%
Benzotriazole 0.3%～0.4%
Tolyltriazole 0.2%～0.3%
Hydrochloric acid 1.5%～1.7%
Nitric acid 33%～36%
Residue is water.
2. metal scavenger composition according to claim 1 is characterized in that the acid equivalent of described metal scavenger composition is greater than 6.5N.
3. metal scavenger composition according to claim 1 is characterized in that, wherein the content of iron nitrate is 16.1%.
4. metal scavenger composition according to claim 1 is characterized in that, wherein content of urea is 0.4%.
5. metal scavenger composition according to claim 1 is characterized in that, wherein the content of benzotriazole is 0.4%.
6. metal scavenger composition according to claim 1 is characterized in that, wherein the content of tolyltriazole is 0.3%.
7. metal scavenger composition according to claim 1 is characterized in that, wherein the content of hydrochloric acid is 1.6%.
8. metal scavenger composition according to claim 1 is characterized in that, wherein the content of nitric acid is 35%.
9. metal scavenger composition according to claim 1 is characterized in that, wherein the content of water is 46.2%.
10. according to claim 1 or 9 described metal scavenger compositions, it is characterized in that wet concentration wherein is tap water, distilled water, deionized water or softening water naturally.
11. metal scavenger composition according to claim 10 is characterized in that, wet concentration wherein is tap water naturally.
12. a method of producing the described metal scavenger composition of claim 1 comprises the steps:
Under the normal temperature and pressure
(1) in producing groove, proportionally adds starting material nitric acid, iron nitrate, hydrochloric acid, urea, benzotriazole, tolyltriazole and water successively;
(2) test after the dissolving through being stirred to fully.
Inspecting standard: proportion (25 ℃): 1.26+/-0.02
Acid equivalent:＞6.5N
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100309068A CN100537848C (en) | 2007-10-18 | 2007-10-18 | A kind of metal scavenger composition and production method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100309068A CN100537848C (en) | 2007-10-18 | 2007-10-18 | A kind of metal scavenger composition and production method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN101139715A true CN101139715A (en) | 2008-03-12 |
| CN100537848C CN100537848C (en) | 2009-09-09 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB2007100309068A Expired - Fee Related CN100537848C (en) | 2007-10-18 | 2007-10-18 | A kind of metal scavenger composition and production method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102507571A (en) * | 2011-11-02 | 2012-06-20 | 苏州华碧微科检测技术有限公司 | Chemical analysis method for lead elements in tin-lead alloy solder |
| CN104149015A (en) * | 2012-11-23 | 2014-11-19 | 江苏顺发电热材料有限公司 | Electric heating pipe roller burnishing treatment process |
| CN104711573A (en) * | 2015-03-27 | 2015-06-17 | 章平传 | Polyacid composite type solder removing solution |
| CN105714298A (en) * | 2016-03-23 | 2016-06-29 | 广东工业大学 | Tin stripping agent based on sulfuric acid-ferric salt system and preparing method of tin stripping agent |
| CN110408935A (en) * | 2018-04-27 | 2019-11-05 | 惠州市鸿宇泰科技有限公司 | A kind of recycling auxiliary agent of tin removal waste liquor and the method for resource of tin removal waste liquor |
| CN111748817A (en) * | 2020-07-10 | 2020-10-09 | 龙南鸿宇泰科技有限公司 | Tin stripping water additive |
| CN112111741A (en) * | 2020-09-25 | 2020-12-22 | 深圳市祺鑫环保科技有限公司 | Tin stripping liquid copper protecting agent and tin stripping liquid |
-
2007
- 2007-10-18 CN CNB2007100309068A patent/CN100537848C/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102507571A (en) * | 2011-11-02 | 2012-06-20 | 苏州华碧微科检测技术有限公司 | Chemical analysis method for lead elements in tin-lead alloy solder |
| CN104149015A (en) * | 2012-11-23 | 2014-11-19 | 江苏顺发电热材料有限公司 | Electric heating pipe roller burnishing treatment process |
| CN104711573A (en) * | 2015-03-27 | 2015-06-17 | 章平传 | Polyacid composite type solder removing solution |
| CN105714298A (en) * | 2016-03-23 | 2016-06-29 | 广东工业大学 | Tin stripping agent based on sulfuric acid-ferric salt system and preparing method of tin stripping agent |
| CN105714298B (en) * | 2016-03-23 | 2019-01-29 | 广东利尔化学有限公司 | It is a kind of based on sulfuric acid-molysite system etching agent and preparation method thereof |
| CN110408935A (en) * | 2018-04-27 | 2019-11-05 | 惠州市鸿宇泰科技有限公司 | A kind of recycling auxiliary agent of tin removal waste liquor and the method for resource of tin removal waste liquor |
| CN111748817A (en) * | 2020-07-10 | 2020-10-09 | 龙南鸿宇泰科技有限公司 | Tin stripping water additive |
| CN112111741A (en) * | 2020-09-25 | 2020-12-22 | 深圳市祺鑫环保科技有限公司 | Tin stripping liquid copper protecting agent and tin stripping liquid |
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| Publication number | Publication date |
|---|---|
| CN100537848C (en) | 2009-09-09 |
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Address after: 519085 Guangdong city of Zhuhai province Zhuhai international science and Technology Industrial Park Jin Feng Road No. 26 Patentee after: ZHUHAI SHUNZE TECHNOLOGY CO.,LTD. Address before: 519085 Guangdong city of Zhuhai province Zhuhai international science and Technology Industrial Park Jin Feng Road No. 26 Patentee before: Zhuhai Shunze Electronic Co.,Ltd. |
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Granted publication date: 20090909 Termination date: 20211018 |