CN107151028A - A kind of method that utilization alkaline etching liquid produces basic copper sulfate - Google Patents

A kind of method that utilization alkaline etching liquid produces basic copper sulfate Download PDF

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Publication number
CN107151028A
CN107151028A CN201710424162.1A CN201710424162A CN107151028A CN 107151028 A CN107151028 A CN 107151028A CN 201710424162 A CN201710424162 A CN 201710424162A CN 107151028 A CN107151028 A CN 107151028A
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CN
China
Prior art keywords
copper sulfate
basic copper
alkaline etching
etching liquid
copper sulphate
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Application number
CN201710424162.1A
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Chinese (zh)
Inventor
郑绵
彭军
刘春�
周菲
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Jiangmen Dongjiang Environmental Protection Technology Co Ltd
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Jiangmen Dongjiang Environmental Protection Technology Co Ltd
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Priority to CN201710424162.1A priority Critical patent/CN107151028A/en
Publication of CN107151028A publication Critical patent/CN107151028A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G3/00Compounds of copper
    • C01G3/10Sulfates

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • ing And Chemical Polishing (AREA)
  • Manufacturing Of Printed Circuit Boards (AREA)

Abstract

The invention belongs to field of fine chemical, it is related to a kind of method that utilization alkaline etching liquid produces basic copper sulfate.The method of the present invention is pre-processed to copper sulphate mother liquor and etching solution first, and both then are mixed into neutralization, by controlling the temperature and pH of neutralization reaction, satisfactory basic copper sulfate crystal is grown.The processing line of the present invention is short out, and simple to operate, raw material is easy to get, and can reach quantity-produced effect, improves production production capacity.The etching solution of a large amount of copper sulphate mother liquors produced during industrial production copper sulphate and circuit board plant is used as to the raw material of production basic copper sulfate, it provide not only the rate of recovery of copper, add the added value of copper products, storage and the environmental pollution brought and the problem of resource waste of a large amount of copper sulphate mother liquors and etching solution are also solved, meets the theory of environmental protection.

Description

A kind of method that utilization alkaline etching liquid produces basic copper sulfate
Technical field
The invention belongs to field of fine chemical, it is related to a kind of method that utilization etching solution produces basic copper sulfate.
Background technology
Substantial amounts of copper sulphate mother liquor can be produced during industrial production copper sulphate, if without processing, this part is female Liquid can not only take substantial amounts of memory space, can also cause the problems such as environmental pollution and wasting of resources.The etching solution of circuit board plant In containing substantial amounts of copper ion, ammonium ion etc., if be not used, will also result in the problems such as environmental pollution and wasting of resources.
Basic copper sulfate is a kind of widely used chemical reagent, and it is the active ingredient of agricultural chemicals Bordeaux mixture, and bohr Many liquid are widely used in the preventing and treating of crops lesion.In addition, basic copper sulfate is also used as bactericidal agent and insecticide is used.Can be with Basic copper sulfate is produced using following reaction:Cu(NH3)4Cl2+CuSO4→Cu2(OH)2SO4↓+NH4Cl.Wherein, reactant CuSO4The main component of a large amount of copper sulphate mother liquors precisely produced during industrial production copper sulphate, Cu (NH3)4Cl2Just It is the main component of circuit board plant etching solution.The a large amount of copper sulphate that therefore, it can to produce during industrial production copper sulphate are female The etching solution of liquid and circuit board plant is used as the raw material of production basic copper sulfate, can not only solve copper sulphate mother liquor and etching solution institute The problem of bringing, can also provide a kind of advantageously with the downstream product being worth.
The content of the invention
It is an object of the invention to provide a kind of method that utilization etching solution produces basic copper sulfate, industrial production sulphur is solved The problem of etching solution that a large amount of copper sulphate mother liquors and circuit board plant are produced during sour copper is brought.
The purpose of the present invention is achieved through the following technical solutions:
A kind of method that utilization alkaline etching liquid produces basic copper sulfate, comprises the following steps:
(1) copper sulphate mother liquor is pre-processed:Copper sulphate mother liquor is added under pretreatment tank, stirring condition, hydrogen peroxide is added straight It is limpid transparent to mother liquor, magnesium chloride solution reaction 1-2 hours is added, then ammonification water regulation pH, filtering and collecting filter liquid is standby With;
(2) alkaline etching liquid is pre-processed:Alkaline etching liquid is added under pretreatment tank, stirring condition, magnesium chloride is added anti- Answer 1-2 hours, add ammoniacal liquor regulation pH, filtering and collecting filter liquid is standby;
(3) under 70-80r/min stirring condition, the copper sulphate mother liquor of step (1) processing is handled with step (2) Alkaline etching liquid by volume 1:1-1.2 is mixed, and it is 55-65 DEG C to control temperature, and it is 5.0-5.5 to control pH, in making both abundant And reaction, obtain the solution of the crystal containing basic copper sulfate;
(4) solution of filtration step (3) processing, obtains filtrate and collects basic copper sulfate crystal;
(5) the basic copper sulfate crystal for obtaining water and step (4) is by solid-to-liquid ratio 1:1-2 mixing, washings 1-2 times, then mistake Filter collection obtains basic copper sulfate crystal.
Preferably, the concentration of copper sulphate mother liquor described in step (1) is 80-120g/L.
Preferably, regulation pH to 2.0-2.5 in step (1).
Preferably, the concentration of alkaline etching liquid described in step (2) is 50-80g/L.
Preferably, regulation pH to 8.5-9.0 in step (2).
The present invention utilizes a large amount of copper sulphate mother liquors produced during industrial production copper sulphate and the etching solution of circuit board plant Raw material as production basic copper sulfate, the main reaction occurred is Cu (NH3)4Cl2+CuSO4→Cu2(OH)2SO4↓+NH4Cl。 Wherein, in advance by copper sulphate mother liquor dioxygen water process so that the cuprous ion in copper sulphate mother liquor is oxidized to copper ion, so The arsenic added afterwards in magnesium chloride removing copper sulphate mother liquor.A large amount of sulfuric acid have been used during copper sulphate is prepared, sulphur is caused Sour copper mother liquor shows highly acid, it is necessary to add ammoniacal liquor regulation pH to 2.0-2.5.By alkaline etching liquid with being used after magnesium chloride arsenic removal Its pH regulations are arrived 8.5-9.0 by ammoniacal liquor.Copper sulphate mother liquor is mixed into neutralization with etching solution, the pH for controlling neutralization reaction is 5.0- 5.5, temperature is 55-65 DEG C.It ensure that on this condition and obtain superior in quality basic copper sulfate product.Gained filtrate is passed through Copper content is in below 0.5ppm after ion exchange, then handle by evaporator, biochemical regulation processing, cross MBR films and special membrane after, Obtain the waste water of qualified discharge.
Beneficial effects of the present invention:The processing line of the present invention is short out, and simple to operate, raw material is easy to get, and can reach continuous life The effect of production, improves production scale.By a large amount of copper sulphate mother liquors produced during industrial production copper sulphate and circuit board plant Etching solution is used as the raw material of production basic copper sulfate, provide not only the rate of recovery of copper, adds the added value of copper products, also solve Storage and the environmental pollution brought and the problem of resource waste for a large amount of copper sulphate mother liquors and the etching solution of having determined, meet green ring The theory of guarantor.
Embodiment
Embodiment 1
A kind of method that utilization alkaline etching liquid produces basic copper sulfate, comprises the following steps
(1) copper sulphate mother liquor is pre-processed:80g/L copper sulphate mother liquor is added under pretreatment tank, stirring condition, added double Oxygen water is limpid transparent up to mother liquor, adds magnesium chloride solution and reacts 1.5 hours, then ammonification water regulation pH to 2, is received after filtering Collect filtrate standby;
(2) alkaline etching liquid is pre-processed:50g/L alkaline etching liquid is added under pretreatment tank, stirring condition, chlorine is added Change reactive magnesium 1.5 hours, add ammoniacal liquor regulation pH to 8.5, filtering and collecting filter liquid is standby;
(3) under 70-80r/min stirring condition, the copper sulphate mother liquor of step (1) processing is handled with step (2) Alkaline etching liquid by volume 1:1 mixing, it is 55 DEG C to control temperature, and it is 5.0 to control pH, makes both abundant neutralization reactions, obtains The solution of the crystal containing basic copper sulfate;
(4) solution of filtration step (3) processing, obtains filtrate and collects basic copper sulfate crystal;
(5) the basic copper sulfate crystal for obtaining water and step (4) is by solid-to-liquid ratio 1:1.5 mixing, washings 1 time, are then filtered Collection obtains basic copper sulfate crystal.
Embodiment 2
A kind of method that utilization alkaline etching liquid produces basic copper sulfate, comprises the following steps:
(1) copper sulphate mother liquor is pre-processed:100g/L copper sulphate mother liquor is added under pretreatment tank, stirring condition, added Hydrogen peroxide is limpid transparent up to mother liquor, adds magnesium chloride solution reaction 1 hour, then ammonification water regulation pH to 2.2, after filtering Collect filtrate standby;
(2) alkaline etching liquid is pre-processed:65g/L alkaline etching liquid is added under pretreatment tank, stirring condition, chlorine is added Change reactive magnesium 1 hour, add ammoniacal liquor regulation pH to 8.7, filtering and collecting filter liquid is standby;
(3) under 70-80r/min stirring condition, the copper sulphate mother liquor of step (1) processing is handled with step (2) Alkaline etching liquid by volume 1:1.1 mixing, it is 60 DEG C to control temperature, and it is 5.2 to control pH, makes both abundant neutralization reactions, obtains To the solution of the crystal containing basic copper sulfate;
(4) solution of filtration step (3) processing, obtains filtrate and collects basic copper sulfate crystal;
(5) the basic copper sulfate crystal for obtaining water and step (4) is by solid-to-liquid ratio 1:1 mixing, washing 2 times, then filtering is received Collection obtains basic copper sulfate crystal.
Embodiment 3
A kind of method that utilization alkaline etching liquid produces basic copper sulfate, comprises the following steps:
(1) copper sulphate mother liquor is pre-processed:120g/L copper sulphate mother liquor is added under pretreatment tank, stirring condition, added Hydrogen peroxide is limpid transparent up to mother liquor, adds magnesium chloride solution reaction 2 hours, then ammonification water regulation pH to 2.5, after filtering Collect filtrate standby;
(2) alkaline etching liquid is pre-processed:80g/L alkaline etching liquid is added under pretreatment tank, stirring condition, chlorine is added Change reactive magnesium 2 hours, add ammoniacal liquor regulation pH to 9.0, filtering and collecting filter liquid is standby;
(3) under 70-80r/min stirring condition, the copper sulphate mother liquor of step (1) processing is handled with step (2) Alkaline etching liquid by volume 1:1.2 mixing, it is 65 DEG C to control temperature, and it is 5.5 to control pH, makes both abundant neutralization reactions, obtains To the solution of the crystal containing basic copper sulfate;
(4) solution of filtration step (3) processing, obtains filtrate and collects basic copper sulfate crystal;
(5) the basic copper sulfate crystal for obtaining water and step (4) is by solid-to-liquid ratio 1:2 mixing, washings 1 time, then filtering is received Collection obtains basic copper sulfate crystal.

Claims (5)

1. a kind of method that utilization alkaline etching liquid produces basic copper sulfate, it is characterised in that comprise the following steps:
(1) copper sulphate mother liquor is pre-processed:Copper sulphate mother liquor is added under pretreatment tank, stirring condition, hydrogen peroxide is added until female Liquid is limpid transparent, adds magnesium chloride solution reaction 1-2 hours, then ammonification water regulation pH, and filtering and collecting filter liquid is standby;
(2) alkaline etching liquid is pre-processed:Alkaline etching liquid is added under pretreatment tank, stirring condition, magnesium chloride 1-2 is added Hour, ammoniacal liquor regulation pH is added, filtering and collecting filter liquid is standby;
(3) under 70-80r/min stirring condition, the alkalescence that the copper sulphate mother liquor of step (1) processing is handled with step (2) Etching solution by volume 1:1-1.2 is mixed, and it is 55-65 DEG C to control temperature, and it is 5.0-5.5 to control pH, both is fully neutralized instead Should, obtain the solution of the crystal containing basic copper sulfate;
(4) solution of filtration step (3) processing, obtains filtrate and collects basic copper sulfate crystal;
(5) the basic copper sulfate crystal for obtaining water and step (4) is by solid-to-liquid ratio 1:1-2 mixing, washings 1-2 times, then filtering is received Collection obtains basic copper sulfate crystal.
2. the method that utilization alkaline etching liquid according to claim 1 produces basic copper sulfate, it is characterised in that step (1) concentration of the copper sulphate mother liquor is 80-120g/L.
3. the method that utilization alkaline etching liquid according to claim 1 produces basic copper sulfate, it is characterised in that step (1) regulation pH to 2.0-2.5 in.
4. the method that utilization alkaline etching liquid according to claim 1 produces basic copper sulfate, it is characterised in that step (2) concentration of the alkaline etching liquid is 50-80g/L.
5. the method that utilization alkaline etching liquid according to claim 1 produces basic copper sulfate, it is characterised in that step (2) regulation pH to 8.5-9.0 in.
CN201710424162.1A 2017-06-07 2017-06-07 A kind of method that utilization alkaline etching liquid produces basic copper sulfate Pending CN107151028A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113402096A (en) * 2021-06-17 2021-09-17 遂宁市星河环境技术有限公司 Stripping and hanging waste liquid treatment method for PCB factory

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102602980A (en) * 2012-04-25 2012-07-25 廖勇志 Industrial preparation method of alkali copper sulfate

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102602980A (en) * 2012-04-25 2012-07-25 廖勇志 Industrial preparation method of alkali copper sulfate

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113402096A (en) * 2021-06-17 2021-09-17 遂宁市星河环境技术有限公司 Stripping and hanging waste liquid treatment method for PCB factory

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Application publication date: 20170912