CN101780972B - Method for preparing basic bluestone by utilizing PCB ammonium persulfate-H2SO4 micro-etched waste liquid - Google Patents
Method for preparing basic bluestone by utilizing PCB ammonium persulfate-H2SO4 micro-etched waste liquid Download PDFInfo
- Publication number
- CN101780972B CN101780972B CN2010101171199A CN201010117119A CN101780972B CN 101780972 B CN101780972 B CN 101780972B CN 2010101171199 A CN2010101171199 A CN 2010101171199A CN 201010117119 A CN201010117119 A CN 201010117119A CN 101780972 B CN101780972 B CN 101780972B
- Authority
- CN
- China
- Prior art keywords
- micro
- waste liquid
- reaction kettle
- etched waste
- ammonia still
- Prior art date
- Legal status (The legal status 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 status listed.)
- Expired - Fee Related
Links
- 238000000034 method Methods 0.000 title claims abstract description 53
- 239000002699 waste material Substances 0.000 title claims abstract description 39
- 239000007788 liquid Substances 0.000 title claims abstract description 37
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 title claims abstract description 30
- 229910000366 copper(II) sulfate Inorganic materials 0.000 title abstract 5
- JZCCFEFSEZPSOG-UHFFFAOYSA-L copper(II) sulfate pentahydrate Chemical compound O.O.O.O.O.[Cu+2].[O-]S([O-])(=O)=O JZCCFEFSEZPSOG-UHFFFAOYSA-L 0.000 title abstract 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 88
- 238000006243 chemical reaction Methods 0.000 claims abstract description 58
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 44
- 239000010949 copper Substances 0.000 claims abstract description 25
- 238000003756 stirring Methods 0.000 claims abstract description 18
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910052802 copper Inorganic materials 0.000 claims abstract description 17
- 238000001914 filtration Methods 0.000 claims abstract description 12
- 239000002244 precipitate Substances 0.000 claims abstract description 11
- 238000005406 washing Methods 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 48
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 21
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 21
- 229910021653 sulphate ion Inorganic materials 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000013019 agitation Methods 0.000 claims description 9
- 238000010992 reflux Methods 0.000 claims description 8
- 238000009987 spinning Methods 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 7
- 238000003860 storage Methods 0.000 claims description 6
- 206010013786 Dry skin Diseases 0.000 claims 2
- 239000000047 product Substances 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 4
- 238000006386 neutralization reaction Methods 0.000 abstract description 3
- 238000004821 distillation Methods 0.000 abstract description 2
- 239000003637 basic solution Substances 0.000 abstract 2
- 238000001704 evaporation Methods 0.000 abstract 2
- 230000008020 evaporation Effects 0.000 abstract 2
- 239000000706 filtrate Substances 0.000 abstract 2
- 230000003472 neutralizing effect Effects 0.000 abstract 2
- 230000001276 controlling effect Effects 0.000 abstract 1
- 239000002270 dispersing agent Substances 0.000 abstract 1
- 239000006193 liquid solution Substances 0.000 abstract 1
- 238000004064 recycling Methods 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 10
- 235000011114 ammonium hydroxide Nutrition 0.000 description 6
- 238000003556 assay Methods 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 239000002245 particle Substances 0.000 description 4
- 239000002351 wastewater Substances 0.000 description 4
- VHSHLMUCYSAUQU-UHFFFAOYSA-N 2-hydroxypropyl methacrylate Chemical compound CC(O)COC(=O)C(C)=C VHSHLMUCYSAUQU-UHFFFAOYSA-N 0.000 description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 229920005552 sodium lignosulfonate Polymers 0.000 description 3
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 2
- 235000011941 Tilia x europaea Nutrition 0.000 description 2
- 150000003863 ammonium salts Chemical class 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 239000004571 lime Substances 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- FSLGRPCWSUDGGH-UHFFFAOYSA-N 2-methylnaphthalene-1-sulfonic acid;sodium Chemical compound [Na].C1=CC=CC2=C(S(O)(=O)=O)C(C)=CC=C21 FSLGRPCWSUDGGH-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 1
- 239000004594 Masterbatch (MB) Substances 0.000 description 1
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 235000011116 calcium hydroxide Nutrition 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000007859 condensation product Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000012851 eutrophication Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 235000011118 potassium hydroxide Nutrition 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
Images
Landscapes
- Removal Of Specific Substances (AREA)
Abstract
The invention discloses a method for preparing basic bluestone by utilizing PCB ammonium persulfate-H2SO4 micro-etched waste liquid. The method comprises the following steps of: (1) preheating ammonium persulfate-H2SO4 micro-etched waste liquid and basic solution to the temperature of between 50 and 100 DEG C respectively, and adding the preheated micro-etched waste liquid into a neutralizing reaction kettle with a stirring device; (2) gradually adding the basic solution into the micro-etched waste liquid with the stirring for neutralization reaction, and controlling the pH value in the neutralizing reaction kettle to be between 8.0 and 13.0; (3) after filtering precipitate, adding dispersant into filtrate; (4) transferring the filtrate of which the pH value is regulated to an ammonia evaporation reaction kettle for atmospheric distillation to ensure that ammonia escapes from the reaction kettle till the pH value is reduced to be between 7.5 and 8.5, and completing ammonia evaporation; and (5) filtering, washing, drying and sifting basic bluestone precipitate in the material to obtain a crystal-type basic bluestone product. The method has the advantages of efficiently recycling copper resource and contributing to generating high-purity basic bluestone, along with simple whole process equipment, easily controlled operating conditions, and less equipment investment.
Description
Technical field:
The present invention relates to a kind of PCB of utilization ammonium persulphate-H
2SO
4Micro-etched waste liquid is produced the method for Basic Chrome Sulphate, belongs to field of fine chemical.
Background technology:
In printed circuit board is produced; The pre-treatment of many operations all needs little erosion; Like holeization (PTH), graphic plating (PP), hot air leveling (HASL) and apply that Organic Solderability protective material (OSP) is preceding all need use micro-etching solution; To remove the microcosmic alligatoring of zone of oxidation and formation on the copper surface, to strengthen the subsequent handling bonding force, more common etching solution mainly contains two kinds at present: a kind of is persulphate-H
2SO
4System, another kind are H
2O
2-H
2SO
4System.And first kind of system often adopts ammonium persulphate-H
2SO
4Solution.
Ammonium persulphate-the H of circuit board plant
2SO
4Micro-etched waste liquid contains Cu
2+, NH
4 +And H
2SO
4, be discharged into waste plant usually and handle the back discharging, and a large amount of copper gets in the mud through materialization, though the sludge incineration meeting is converted into renewable resource with copper, this method organic efficiency is low, energy loss is big.In addition, there is a large amount of NH in the waste water
4 +Ion enters water body and will cause body eutrophication, reduces the water body ornamental value, and the nitrate salt of oxidized generation and growth of nitrite mailbox hydrobiont even human health.
At present, take electrolytic process to handle this waste liquid, its principle is to utilize electrochemistry that electric energy is converted into chemical energy, makes the cupric ion in the waste liquid be converted into a large amount of electric energy of copper simple substance this method consumption, the waste liquid high efficiente callback is not utilized.
Summary of the invention:
The present invention is intended to address the above problem, thereby a kind of PCB of utilization ammonium persulphate-H is provided
2SO
4Micro-etched waste liquid is produced the method for Basic Chrome Sulphate, this method processing efficiency height, effect stability, safe and reliable, suitability by force, can at utmost recycle copper resource and ammonia nitrogen.
To achieve these goals, the invention provides a kind of PCB of utilization ammonium persulphate-H
2SO
4Micro-etched waste liquid is produced the method for Basic Chrome Sulphate, and this method comprises the steps:
(1) with ammonium persulphate-H
2SO
4Micro-etched waste liquid and basic soln are preheating to 50 ~ 100 ℃ respectively, and copper concentration is 10 ~ 50g/L in the micro-etched waste liquid.The micro-etched waste liquid that preheating is good joins in the reaction kettle that has whipping appts, when its add-on finishes for reaction 20% ~ 80% of the material TV;
(2) then, under agitation condition, in above-mentioned micro-etched waste liquid, progressively add basic soln and carry out neutralization reaction, the pH value scope in the control reaction kettle is between 8.0 ~ 13.0.
This reaction equation is following:
H
2SO
4+2NaOH＝Na
2SO
4+2H
2O
(NH
4)
2SO
4+2NaOH≒NH
3·H
2O+Na
2SO
4
4CuSO
4+6NaOH＝Cu
4(OH)
6SO
4↓+3Na
2SO
4
(3) add an amount of dispersion agent behind the filtering precipitate, be used to control Basic Chrome Sulphate crystalline size.Dispersion agent is preferably one or more in the formaldehyde condensation products of X 2073, sodium lignosulfonate, calcium, HPMA, methyl naphthalene sulfonic acid sodium, and consumption is 2% ~ 8% of a masterbatch;
(4) change the filtrating of the above-mentioned pH of mixing up value over to the ammonia still process reaction kettle and carry out air distillation ammonia is therefrom overflowed, reduce to 7.5 ~ 8.5, finish ammonia still process to the pH value; The ammonia still process temperature is 60 ~ 100 ℃, and the ammonia still process time is 0.5 ~ 3.5h; The ammonia used water that steams, a kind of absorption in the excessive dilute sulphuric acid obtain ammoniacal liquor or ammonium salt product;
(5) Basic Chrome Sulphate in material deposition is again through filtering, washing, drying, obtaining crystal type Basic Chrome Sulphate product after sieving.
In the step (1), described basic soln is one of NaOH, KOH, ammoniacal liquor, slaked lime (emulsion) of different concns or their two kinds or multiple mixture.
In step (2) and the step (4), the pH value in employing pH electrode The real time measure neutralization reaction still, the ammonia still process reaction kettle is also controlled the add-on and the ammonia still process time of basic soln in view of the above;
In the step (3), add an amount of dispersion agent and be used to control Basic Chrome Sulphate particulate growth particle diameter, make the Basic Chrome Sulphate particle of different-grain diameter.
In the step (5), the drying temperature when dry is 40 ~ 80 ℃.
Compared with prior art, the present invention has following beneficial effect:
(1) the present invention utilizes PCB ammonium persulphate-H for the first time
2SO
4Micro-etched waste liquid prepares Basic Chrome Sulphate as raw material, and the present invention utilizes copper resource, the ammonia resource in the waste liquid, production main products Basic Chrome Sulphate, auxiliary product ammoniacal liquor or ammonium salt, and it is precious changing refuse.
(2) after the present invention recycled through ammonia nitrogen, ammonia nitrogen concentration reduced greatly in the waste water, has alleviated the burden of subsequent waste water materialization or biochemical treatment, and water quality treatment reaches national composite wastewater emission standard easily.
(3) processing unit of the present invention is simple, processing efficiency is high, safe and reliable, not only solved PCB ammonium persulphate-H
2SO
4The processing of micro-etched waste liquid, and realized the resource circulation utilization, reduced copper greatly to natural harm.
(4) may command Basic Chrome Sulphate particulate of the present invention growth particle diameter makes the Basic Chrome Sulphate superfine particle of different-grain diameter.
Description of drawings:
Fig. 1 utilizes ammonium persulphate-H
2SO
4Micro-etched waste liquid is produced the schema of Basic Chrome Sulphate.
Embodiment:
Embodiment 1:
At 8M
3Enamel reaction still in add ammonium persulphate-H of copper content 25g/L
2SO
4Micro-etched waste liquid 6M
3, the limit feeds the stirring of steam limit and makes ammonium persulphate-H
2SO
4Micro-etched waste liquid is preheating to 75 ℃.Sodium hydroxide solution with 30% (massfraction) is preheated to 70 ℃ in the raw material storage tank in addition.Start the reaction kettle stirring rake, open the feedstock pump of sodium hydroxide simultaneously and adjust the under meter flow velocity, sodium hydroxide solution is joined in the reaction kettle with the speed of 20L/Min, the pH value of control reaction kettle internal reaction thing is 9.5; Add the 1000g X 2073 behind the filtering precipitate; Change the ammonia still process reaction kettle over to, the ammonia still process that under agitation condition, refluxes, control ammonia still process temperature is at 70 ℃; Reduce to 7.5 to the pH value; End ammonia still process is filtered and with water washing three times, spinning is after 60 ℃ of dry 259 kilograms in light green Basic Chrome Sulphate powder that get.The sample assay is with Cu
4(OH)
6SO
4Count 98.6%.
Embodiment 2:
At 8M
3Enamel reaction still in add ammonium persulphate-H of copper content 50g/L
2SO
4Micro-etched waste liquid 6M
3, the limit feeds the stirring of steam limit and makes ammonium persulphate-H
2SO
4Micro-etched waste liquid is preheating to 75 ℃.Sodium hydroxide solution with 30% (massfraction) is preheated to 70 ℃ in the raw material storage tank in addition.Start the reaction kettle stirring rake, open the feedstock pump of sodium hydroxide simultaneously and adjust the under meter flow velocity, sodium hydroxide solution is joined in the reaction kettle with the speed of 20L/Min, the pH value of control reaction kettle internal reaction thing is 9.5; Add the 1000g X 2073 behind the filtering precipitate; Change the ammonia still process reaction kettle over to, the ammonia still process that under agitation condition, refluxes, control ammonia still process temperature is at 70 ℃; Reduce to 8 to the pH value; End ammonia still process is filtered and with water washing three times, spinning is after 60 ℃ of dry 521 kilograms in light green Basic Chrome Sulphate powder that get.The sample assay is with Cu
4(OH)
6SO
4Count 98.4%.
Embodiment 3:
At 8M
3Enamel reaction still in add ammonium persulphate-H of copper content 35g/L
2SO
4Micro-etched waste liquid 6M
3, the limit feeds the stirring of steam limit and makes ammonium persulphate-H
2SO
4Micro-etched waste liquid is preheating to 50 ℃.Sodium hydroxide solution with 30% (massfraction) is preheated to 50 ℃ in the raw material storage tank in addition.Start the reaction kettle stirring rake, open the feedstock pump of sodium hydroxide simultaneously and adjust the under meter flow velocity, sodium hydroxide solution is joined in the reaction kettle with the speed of 20L/Min, the pH value of control reaction kettle internal reaction thing is 10; Add the 2500g sodium lignosulfonate behind the filtering precipitate; Change the ammonia still process reaction kettle over to, the ammonia still process that under agitation condition, refluxes, control ammonia still process temperature is at 75 ℃; Reduce to 7.5 to the pH value; End ammonia still process is filtered and with water washing three times, spinning is after 60 ℃ of dry 381 kilograms in light green Basic Chrome Sulphate powder that get.The sample assay is with Cu
4(OH)
6SO
4Count 97.6%.
Embodiment 4:
At 8M
3Enamel reaction still in add ammonium persulphate-H of copper content 25g/L
2SO
4Micro-etched waste liquid 6M
3, the limit feeds the stirring of steam limit and makes ammonium persulphate-H
2SO
4Micro-etched waste liquid is preheating to 75 ℃.Ammoniacal liquor with 10% (massfraction) is preheated to 70 ℃ in the raw material storage tank in addition.Start the reaction kettle stirring rake, open the feedstock pump of ammoniacal liquor simultaneously and adjust the under meter flow velocity, ammoniacal liquor is joined in the reaction kettle with the speed of 20L/Min, the pH value scope of control reaction kettle internal reaction thing is 10; Add the 2500g sodium lignosulfonate behind the filtering precipitate; Change the ammonia still process reaction kettle over to, the ammonia still process that under agitation condition, refluxes, control ammonia still process temperature is at 73 ℃; Reduce to 8.0 to the pH value; End ammonia still process is filtered and with water washing three times, spinning is after 60 ℃ of dry 261 kilograms in light green Basic Chrome Sulphate powder that get.The sample assay is with Cu
4(OH)
6SO
4Count 98.0%.
Embodiment 5:
At 8M
3Enamel reaction still in add ammonium persulphate-H of copper content 25g/L
2SO
4Micro-etched waste liquid 6M
3, the limit feeds the stirring of steam limit and makes ammonium persulphate-H
2SO
4Micro-etched waste liquid is preheating to 75 ℃.Start the reaction kettle stirring rake, simultaneously white lime is joined in the reaction kettle, the pH value of control reaction kettle internal reaction thing is 10.5; Add the 1800g HPMA behind the filtering precipitate; Change the ammonia still process reaction kettle over to, the ammonia still process that under agitation condition, refluxes, control ammonia still process temperature is at 75 ℃; Reduce to 8.0 to the pH value; End ammonia still process is filtered and with water washing three times, spinning is after 40 ℃ of dry 265 kilograms in light green Basic Chrome Sulphate powder that get.The sample assay is with Cu
4(OH)
6SO
4Count 96.1%.
Embodiment 6:
At 8M
3Enamel reaction still in add ammonium persulphate-H of copper content 25g/L
2SO
4Micro-etched waste liquid 6M
3, the limit feeds the stirring of steam limit and makes ammonium persulphate-H
2SO
4Micro-etched waste liquid is preheating to 50 ℃.Start the reaction kettle stirring rake, simultaneously white lime is joined in the reaction kettle, the pH value of control reaction kettle internal reaction thing is 10.5; Add the 1800g HPMA behind the filtering precipitate; Change the ammonia still process reaction kettle over to, the ammonia still process that under agitation condition, refluxes, control ammonia still process temperature is at 65 ℃; Reduce to 8.0 to the pH value; End ammonia still process is filtered and with water washing three times, spinning is after 80 ℃ of dry 262 kilograms in light green Basic Chrome Sulphate powder that get.The sample assay is with Cu
4(OH)
6SO
4Count 96.9%.
Claims (1)
1. one kind is utilized PCB ammonium persulphate-H
2SO
4Micro-etched waste liquid is produced the method for Basic Chrome Sulphate, it is characterized in that, comprises the steps:
At 8M
3Enamel reaction still in add ammonium persulphate-H of copper content 25g/L
2SO
4Micro-etched waste liquid 6M
3, the limit feeds the stirring of steam limit and makes ammonium persulphate-H
2SO
4Micro-etched waste liquid is preheating to 75 ℃; Sodium hydroxide solution with 30% massfraction is preheated to 70 ℃ in the raw material storage tank in addition; Start the reaction kettle stirring rake, open the feedstock pump of sodium hydroxide simultaneously and adjust the under meter flow velocity, sodium hydroxide solution is joined in the reaction kettle with the speed of 20L/Min, the pH value of control reaction kettle internal reaction thing is 9.5; Add the 1000g X 2073 behind the filtering precipitate, change the ammonia still process reaction kettle over to, ammonia still process refluxes under agitation condition; Control ammonia still process temperature reduces to 7.5 at 70 ℃ to the pH value, finishes ammonia still process; Filter and with water washing three times, spinning is after 60 ℃ of dryings;
Or at 8M
3Enamel reaction still in add ammonium persulphate-H of copper content 50g/L
2SO
4Micro-etched waste liquid 6M
3, the limit feeds the stirring of steam limit and makes ammonium persulphate-H
2SO
4Micro-etched waste liquid is preheating to 75 ℃; Sodium hydroxide solution with 30% massfraction is preheated to 70 ℃ in the raw material storage tank in addition; Start the reaction kettle stirring rake, open the feedstock pump of sodium hydroxide simultaneously and adjust the under meter flow velocity, sodium hydroxide solution is joined in the reaction kettle with the speed of 20L/Min, the pH value of control reaction kettle internal reaction thing is 9.5; Add the 1000g X 2073 behind the filtering precipitate, change the ammonia still process reaction kettle over to, the ammonia still process that under agitation condition, refluxes, control ammonia still process temperature reduces to 8 at 70 ℃ to the pH value, and end ammonia still process is filtered and with water washing three times, spinning is after 60 ℃ of dryings.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101171199A CN101780972B (en) | 2010-02-23 | 2010-02-23 | Method for preparing basic bluestone by utilizing PCB ammonium persulfate-H2SO4 micro-etched waste liquid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101171199A CN101780972B (en) | 2010-02-23 | 2010-02-23 | Method for preparing basic bluestone by utilizing PCB ammonium persulfate-H2SO4 micro-etched waste liquid |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101780972A CN101780972A (en) | 2010-07-21 |
| CN101780972B true CN101780972B (en) | 2012-02-29 |
Family
ID=42521142
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010101171199A Expired - Fee Related CN101780972B (en) | 2010-02-23 | 2010-02-23 | Method for preparing basic bluestone by utilizing PCB ammonium persulfate-H2SO4 micro-etched waste liquid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101780972B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102815740B (en) * | 2012-08-03 | 2015-04-22 | 西北矿冶研究院 | Production method for improving copper sulfate grade |
| CN103435092B (en) * | 2013-09-01 | 2015-06-24 | 深圳市危险废物处理站有限公司 | Resource recovery method of sodium persulfate-sulfuric acid serial copper-containing microetch waste liquor for PCB (Printed Circuit Board) |
| CN103449501B (en) * | 2013-09-01 | 2015-11-18 | 深圳市危险废物处理站有限公司 | The method of comprehensive utilization of waste liquor in production of basic cupric carbonate |
| CN113402096B (en) * | 2021-06-17 | 2023-04-07 | 遂宁市星河环境技术有限公司 | Stripping and hanging waste liquid treatment method for PCB factory |
-
2010
- 2010-02-23 CN CN2010101171199A patent/CN101780972B/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN101780972A (en) | 2010-07-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103351020B (en) | A kind of production method of basic copper chloride | |
| CN106830030B (en) | A kind of method using the safe and efficient production sandy alumina of aluminium ash | |
| CN102491402B (en) | Method for producing refined copper oxide by utilizing acidic waste etching solution | |
| CN101503762B (en) | Desulphurization and vanadium extraction technique for calcinated vanadium ore | |
| CN108341424A (en) | The production method of copper sulphate | |
| CN103922416A (en) | Method for separating and recovering iron from red mud | |
| CN103145160B (en) | Method for producing alumina by using high-alumina fly ash | |
| CN103693670B (en) | Production method of calcium sulphate dehydrate and production device thereof | |
| CN101643236A (en) | Production of zinc oxide by ammonia water circulation method | |
| CN102703905B (en) | Process for comprehensively utilizing waste tin-stripping solution | |
| CN104944400A (en) | Technology for preparing iron phosphate through hydrolytic method | |
| CN101780972B (en) | Method for preparing basic bluestone by utilizing PCB ammonium persulfate-H2SO4 micro-etched waste liquid | |
| CN102583819B (en) | Method for processing waste water generated by extracting copper oxide from acidic corrosion waste fluid | |
| CN101708835B (en) | Production method of high-purity zinc phosphate | |
| CN103224221A (en) | Method for separating sulfuric acid and ferrous sulfate by using ferrous sulfate monohydrate residue | |
| CN101428841A (en) | Process for producing basic copper carbonate | |
| CN102145904A (en) | Method for extracting alumina from fly ash | |
| CN105129838A (en) | Method for producing copper sulphate by using copper-containing waste solution of PCB circuit board plant | |
| CN101891256B (en) | Production technique of high-purity potassium permanganate and manganese dioxide, and carbon dioxide reaction tower | |
| CN103288286A (en) | Catalytic oxidation treatment method for desulfurized waste liquid | |
| CN104762478A (en) | Method for production and recovery of precious metals on the basis of pickling sludge | |
| CN114906830A (en) | Method for controllably preparing battery-grade iron phosphate from pyrite cinder | |
| CN103601228A (en) | Method for preparation of chemical raw materials by use of fly ash as raw material | |
| CN101525752B (en) | Clean production method for high-purity cobaltosic oxide powder | |
| CN101585522A (en) | Method for recovering phosphorus from urban mud anaerobic digestion solution |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20120229 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |