CN102807277A - Method for removing lead from alkaline etching waste liquid of printed circuit boards - Google Patents

Method for removing lead from alkaline etching waste liquid of printed circuit boards Download PDF

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Publication number
CN102807277A
CN102807277A CN2012102789501A CN201210278950A CN102807277A CN 102807277 A CN102807277 A CN 102807277A CN 2012102789501 A CN2012102789501 A CN 2012102789501A CN 201210278950 A CN201210278950 A CN 201210278950A CN 102807277 A CN102807277 A CN 102807277A
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China
Prior art keywords
waste liquid
alkaline etching
etching waste
lead
liquid
Prior art date
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Pending
Application number
CN2012102789501A
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Chinese (zh)
Inventor
谢逢春
张嫔
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
HUIZHOU DAYAWAN HUILU ENVIRONMENT PROTECTION SERVICE CO Ltd
South China University of Technology SCUT
Original Assignee
HUIZHOU DAYAWAN HUILU ENVIRONMENT PROTECTION SERVICE CO Ltd
South China University of Technology SCUT
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Application filed by HUIZHOU DAYAWAN HUILU ENVIRONMENT PROTECTION SERVICE CO Ltd, South China University of Technology SCUT filed Critical HUIZHOU DAYAWAN HUILU ENVIRONMENT PROTECTION SERVICE CO Ltd
Priority to CN2012102789501A priority Critical patent/CN102807277A/en
Publication of CN102807277A publication Critical patent/CN102807277A/en
Pending legal-status Critical Current

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  • Removal Of Specific Substances (AREA)

Abstract

The invention provides a method for removing lead from alkaline etching waste liquid of printed circuit boards. The method can be used for resource recovery and innocent treatment of alkaline etching waste liquid and belongs to the technical field of chemical industry. The method includes firstly, preparing two-valence-ferrous-free ferric hydroxide precipitant which is easy to precipitate and filter; secondly, adding sulfate solution to alkaline etching waste liquid to be subjected to lead removal, adding the prepared ferric hydroxide precipitant, and fully mixing; and thirdly, performing solid-liquid separation to obtain solid-phase ferric hydroxide precipitant containing lead sulfate to recycle. The obtained liquid phase is alkaline etching waste liquid meeting the requirement for lead content. The method has the advantages treatment cost is low, treating process is simple, treating effect is good, treating efficiency is high, material can be recycled and is environment-friendly and zero-emission, investment on devices is low, and the like. The method is suitable for lead removal of alkaline etching waste liquid.

Description

A kind of from alkaline etching waste liquid for producing printed circuit board the method for deleading
[technical field]
The present invention relates to a kind of from alkaline etching waste liquid for producing printed circuit board the method for deleading, can be used for resource utilization, the innocent treatment procedure of alkaline etching waste liquid for producing, belong to environmental technology field.
[background technology]
Alkaline etching waste liquid for producing printed circuit board is a kind of waste of making the etch process generation of printed circuit board; Wherein mainly contain a large amount of cupric ions and ammonium chloride, ammoniacal liquor; If it is not carried out resource utilization, harmless treatment, then cause than serious environmental and pollute and the wasting of resources.Present resource utilization, method for innocent treatment mainly are as the raw material of producing Chemicals such as copper sulfate, basic copper chloride, cupric oxide with it.And make the plumbous impurity that often contains 50-100ppm in the alkaline etching waste liquid for producing that produces in the process of slicker solder printed circuit board.And as copper sulfate, basic copper chloride that fodder additives is used its lead tolerance is often required very sternly, require lead tolerance to be lower than 10ppm like feed-grade bluestone standard HG2932.If be raw material production feed grade mantoquita as raw material therefore, just must make its product reach requirement by degree of depth deleading with this etching waste liquor.
Existing from alkaline etching waste liquid for producing the deleading technology comprise extraction process method, ion exchange method, the precipitator method etc., these methods are owing to have complex process, cost high, efficient is low, produces defectives such as leaded refuse, does not all reach ideal deleading effect.Therefore be necessary to set up one processing cost be low, treatment capacity big, plumbous removal method in the alkaline etching waste liquid for producing of treatment process, green, environmental protection, being used for leaded etching waste liquor is the production process of the mantoquita used of the fodder additives of raw material.
[summary of the invention]
The objective of the invention is to effectively solve the removal problem of iron contamination in the above-mentioned alkaline etching waste liquid for producing.Traditional precipitator method are to add vitriol earlier the plumbous lead sulfate that generates is precipitated, and then through solid-liquid separation iron are removed.But at this moment often generate the lead sulfate colloidal solid, this colloidal solid volume is little, and specific surface is big; Thereby surface energy is higher, and solubleness is bigger than normal, and lead sulfate can not be precipitated fully; But also make solution solid-liquid separation difficulty, thereby this method for removing lead is difficult to reach the ideal effect.
If but add at this moment the specific surface prepared less, be puffy, be easy to filtering ferric hydroxide precipitate, then formed the colloidal lead sulfate and be adsorbed and flocculation sediment very soon.And this lead sulfate that is adsorbed will be converted into more stable deposit seeds after after a while, and this deposit seeds also can induce the colloid of other lead sulfate to change same stable lead sulfate deposit seeds into.If the ferric hydroxide precipitate of the sulfur-bearing lead plumbate that therefore obtains through solid-liquid separation is used further to the deleading process, can reach very ideal deleading effect.Thereby this method owing to recycle leaded waste, thereby do not have leaded waste discharge.After repeatedly circulating,, can carry out plumbous recycling when lead tolerance runs up to a certain degree.
Therefore present method can be divided into following steps:
1, preparation ferric hydroxide precipitate.
2, sulfate liquor is added the alkaline etching waste liquid for producing of treating deleading.
3, add the ferric hydroxide precipitate for preparing, and fully stir.
4, solid-liquid separation, the solid phase hydrogen iron oxide precipitation of the sulfur-bearing lead plumbate that obtains recycles.The liquid phase that obtains is lead tolerance and meets the requirements of alkaline etching waste liquid for producing.
Characteristics such as present method has that processing cost is low, treating processes is simple, treatment effect is good, processing efficiency is high, and material recycles, green, environmental protection, green, environmental protection, zero release, facility investment are little are well suited for and alkaline etching waste liquid for producing is carried out deleading handle.
[embodiment]
Further specify embodiment of the present invention and effect with following indefiniteness embodiment:
Embodiment 1
The alkaline etching waste liquid for producing lead tolerance of certain circuit board plant is 80ppm, and its deleading treating processes is following:
1, under abundant stirring state, in the liquor ferri trichloridi of the iron hydroxide solution adding 5% with 5%, the control endpoint pH is 7; Add simultaneously ydrogen peroxide 50 will be wherein ferrous iron all be oxidized to ferric iron, churning time is 2 hours, generates to be puffy, to be easy to sedimentation and filtering ferric hydroxide precipitate; And water rinsing repeatedly, flush away sodium-chlor wherein is after waiting to precipitate sedimentation; Discard the upper strata stillness of night, obtain water ratio and be 95% ironic hydroxide slurries.
2, under abundant stirring state, the adding of 10% metabisulfite solution is treated in the alkaline etching waste liquid for producing of deleading that add-on is 10L/m 3, stir half a hour.
3, under abundant stirring state, add the above-mentioned slurries that prepare ferric hydroxide precipitate again, add-on is 5.5L/m 3, stirred 1 hour.
4, carry out solid-liquid separation, the solid phase that obtains recycles as ferric hydroxide precipitate after adding water slurrying.The liquid phase that obtains is lead tolerance and meets the requirements of alkaline etching waste liquid for producing.
Handling the alkaline etching waste liquid for producing lead tolerance that obtains through above-mentioned steps is 5.2ppm, has reached the requirement of production feed grade mantoquita.
Embodiment 2
The alkaline etching waste liquid for producing lead tolerance of certain circuit board plant is 50ppm, and its deleading treating processes is following:
1, under abundant stirring state, the adding of 10% potassium sulfate solution is treated in the alkaline etching waste liquid for producing of deleading that add-on is 12L/m 3, stir half a hour.
2, under abundant stirring state, add again last time the deleading solid-liquid separation and the water cut that adds water slurrying be the slurries of 90% ferric hydroxide precipitate, add-on is 4.2L/m 3, stirred 1 hour.
3, carry out solid-liquid separation, the solid phase that obtains recycles as ferric hydroxide precipitate after adding water slurrying.The liquid phase that obtains is lead tolerance and meets the requirements of alkaline etching waste liquid for producing.
Handling the alkaline etching waste liquid for producing lead tolerance that obtains through above-mentioned steps is 3.2ppm, has reached the requirement of production feed grade mantoquita.
Embodiment 3
The alkaline etching waste liquid for producing lead tolerance of certain circuit board plant is 50ppm, and its deleading treating processes is following:
1, under abundant stirring state, the adding of 10% ammoniumsulphate soln is treated in the alkaline etching waste liquid for producing of deleading that add-on is 8L/m 3, stir half a hour.
2, under abundant stirring state, add again last time the deleading solid-liquid separation and the water cut that adds water slurrying be the slurries of 90% ferric hydroxide precipitate, add-on is 3.5L/m 3, stirred 1 hour.
3,, carry out solid-liquid separation, the solid phase that obtains recycles as ferric hydroxide precipitate after adding water slurrying.The liquid phase that obtains is lead tolerance and meets the requirements of alkaline etching waste liquid for producing.
Handling the alkaline etching waste liquid for producing lead tolerance that obtains through above-mentioned steps is 4.3ppm, has reached the requirement of production feed grade mantoquita.
Above-described embodiment has only expressed preferred implementation of the present invention, can not be interpreted as the restriction to claim of the present invention, so the present invention is not limited to this concrete technical process.Those skilled in the art can also make some distortion and improvement according to technical scheme of the present invention and design, and these all belong to protection scope of the present invention.So all other embodiments that the claim scope draws according to the present invention all should belong to the scope that the present invention is contained.

Claims (3)

1. the method for a deleading from alkaline etching waste liquid for producing printed circuit board is characterized in that comprising following steps:
(1), preparation be easy to sedimentation and filtering, do not contain ferrous ferric hydroxide precipitate.
(2), sulfate liquor is added the alkaline etching waste liquid for producing of treating deleading.
(3), add the ferric hydroxide precipitate prepare, and fully stir.
(4), solid-liquid separation, the sulfur-bearing lead plumbate solid phase hydrogen iron oxide precipitation that obtains recycles.The liquid phase that obtains is lead tolerance and meets the requirements of alkaline etching waste liquid for producing.
2. treatment process according to claim 1 is characterized in that: the vitriol in said (2) step can be sodium sulfate, vitriolate of tartar, ammonium sulfate, copper sulfate or other soluble sulphates.
3. treatment process according to claim 1 is characterized in that: said (4) step solid-liquid separation is separated with the method for press filtration, or separates with other solid-liquid separating methods.
CN2012102789501A 2012-08-07 2012-08-07 Method for removing lead from alkaline etching waste liquid of printed circuit boards Pending CN102807277A (en)

Priority Applications (1)

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CN2012102789501A CN102807277A (en) 2012-08-07 2012-08-07 Method for removing lead from alkaline etching waste liquid of printed circuit boards

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Application Number Priority Date Filing Date Title
CN2012102789501A CN102807277A (en) 2012-08-07 2012-08-07 Method for removing lead from alkaline etching waste liquid of printed circuit boards

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106966469A (en) * 2017-04-10 2017-07-21 中国铝业股份有限公司 A kind of processing method of containing sulfate radicals waste water

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
《冶金分析》 20071231 徐红波等 "碳酸钙和氢氧化铁共沉淀脱除碱性蚀刻液中铅砷" 第46-49页 1-3 第27卷, 第12期 *
徐红波等: ""碳酸钙和氢氧化铁共沉淀脱除碱性蚀刻液中铅砷"", 《冶金分析》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106966469A (en) * 2017-04-10 2017-07-21 中国铝业股份有限公司 A kind of processing method of containing sulfate radicals waste water

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Application publication date: 20121205