CN101780972A - 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
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- CN101780972A CN101780972A CN201010117119A CN201010117119A CN101780972A CN 101780972 A CN101780972 A CN 101780972A CN 201010117119 A CN201010117119 A CN 201010117119A CN 201010117119 A CN201010117119 A CN 201010117119A CN 101780972 A CN101780972 A CN 101780972A
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- micro
- waste liquid
- etched waste
- basic
- ammonium persulphate
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Links
- 238000000034 method Methods 0.000 title claims abstract description 59
- 239000002699 waste material Substances 0.000 title claims abstract description 48
- 239000007788 liquid Substances 0.000 title claims abstract description 44
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 title claims abstract description 37
- 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
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 44
- 239000010949 copper Substances 0.000 claims abstract description 24
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052802 copper Inorganic materials 0.000 claims abstract description 16
- 238000001914 filtration Methods 0.000 claims abstract description 12
- 239000003637 basic solution Substances 0.000 claims abstract description 10
- 239000002244 precipitate Substances 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims abstract description 9
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 7
- 239000000463 material Substances 0.000 claims abstract description 6
- 239000000047 product Substances 0.000 claims abstract description 6
- 239000000706 filtrate Substances 0.000 claims abstract description 4
- 238000004821 distillation Methods 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 claims abstract description 3
- 239000006193 liquid solution Substances 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 33
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 31
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 31
- 229910021653 sulphate ion Inorganic materials 0.000 claims description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 238000013019 agitation Methods 0.000 claims description 8
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 7
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 239000006185 dispersion Substances 0.000 claims description 5
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 4
- 230000003301 hydrolyzing effect Effects 0.000 claims description 4
- 229920000141 poly(maleic anhydride) Polymers 0.000 claims description 4
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 4
- 229920005552 sodium lignosulfonate Polymers 0.000 claims description 4
- 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 claims description 2
- 239000004594 Masterbatch (MB) Substances 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 2
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 2
- 239000000920 calcium hydroxide Substances 0.000 claims description 2
- 235000011116 calcium hydroxide Nutrition 0.000 claims description 2
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 2
- 239000007859 condensation product Substances 0.000 claims description 2
- 239000013078 crystal Substances 0.000 claims description 2
- 230000001186 cumulative effect Effects 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 238000001556 precipitation Methods 0.000 claims description 2
- 238000007873 sieving Methods 0.000 claims description 2
- 239000001117 sulphuric acid Substances 0.000 claims description 2
- 235000011149 sulphuric acid Nutrition 0.000 claims description 2
- 238000003756 stirring Methods 0.000 abstract description 14
- 238000001704 evaporation Methods 0.000 abstract 2
- 230000008020 evaporation Effects 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
- 238000004064 recycling Methods 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 10
- 239000000243 solution Substances 0.000 description 9
- 238000003556 assay Methods 0.000 description 6
- 238000005119 centrifugation Methods 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 238000010992 reflux Methods 0.000 description 6
- 239000002994 raw material Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 4
- 239000002351 wastewater Substances 0.000 description 4
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 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
- 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
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 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
- 239000002131 composite material Substances 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
- 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
- 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
- 239000010802 sludge Substances 0.000 description 1
Images
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 microetch; as holeization (PTH), graphic plating (PP), hot air leveling (HASL) and apply that Organic Solderability protective material (OSP) is preceding all to need to 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 enters 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 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 strong, 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 solution 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 reactor that has whipping appts, when its add-on finishes for reaction 20% ~ 80% of the material cumulative volume;
(2) then, progressively add basic solution and carry out neutralization reaction under agitation condition in above-mentioned micro-etched waste liquid, the pH value scope in the control reactor is between 8.0 ~ 13.0.
This reaction equation is as follows:
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 Sodium dodecylbenzene sulfonate, sodium lignosulfonate, calcium, hydrolytic polymaleic anhydride, methyl naphthalene sulfonic acid sodium, and consumption is 2% ~ 8% of a masterbatch;
(4) filtrate of the above-mentioned pH of mixing up value is changed over to the ammonia still process reactor 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 precipitation more after filtration, washing, dry, obtain crystal type Basic Chrome Sulphate product after sieving.
In the step (1), described basic solution is one of NaOH, KOH, ammoniacal liquor, slaked lime (emulsion) of different concns or their two kinds or more of 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 reactor is also controlled the add-on and the ammonia still process time of basic solution 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 follow-up waste water physicochemical 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 reactor stirring rake, open the feedstock pump of sodium hydroxide simultaneously and adjust the under meter flow velocity, sodium hydroxide solution is joined in the reactor with the speed of 20L/Min, the pH value of control reactor internal reaction thing is 9.5; Add the 1000g Sodium dodecylbenzene sulfonate behind the filtering precipitate, change the ammonia still process reactor over to, ammonia still process refluxes under agitation condition, 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, centrifugation 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 reactor stirring rake, open the feedstock pump of sodium hydroxide simultaneously and adjust the under meter flow velocity, sodium hydroxide solution is joined in the reactor with the speed of 20L/Min, the pH value of control reactor internal reaction thing is 9.5; Add the 1000g Sodium dodecylbenzene sulfonate behind the filtering precipitate, change the ammonia still process reactor over to, ammonia still process refluxes under agitation condition, 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, centrifugation 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 reactor stirring rake, open the feedstock pump of sodium hydroxide simultaneously and adjust the under meter flow velocity, sodium hydroxide solution is joined in the reactor with the speed of 20L/Min, the pH value of control reactor internal reaction thing is 10; Add the 2500g sodium lignosulfonate behind the filtering precipitate, change the ammonia still process reactor over to, ammonia still process refluxes under agitation condition, 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, centrifugation 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 reactor stirring rake, open the feedstock pump of ammoniacal liquor simultaneously and adjust the under meter flow velocity, ammoniacal liquor is joined in the reactor with the speed of 20L/Min, the pH value scope of control reactor internal reaction thing is 10; Add the 2500g sodium lignosulfonate behind the filtering precipitate, change the ammonia still process reactor over to, ammonia still process refluxes under agitation condition, 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, centrifugation 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 reactor stirring rake, simultaneously white lime is joined in the reactor, the pH value of control reactor internal reaction thing is 10.5; Add the 1800g hydrolytic polymaleic anhydride behind the filtering precipitate, change the ammonia still process reactor over to, ammonia still process refluxes under agitation condition, 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, centrifugation 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 reactor stirring rake, simultaneously white lime is joined in the reactor, the pH value of control reactor internal reaction thing is 10.5; Add the 1800g hydrolytic polymaleic anhydride behind the filtering precipitate, change the ammonia still process reactor over to, ammonia still process refluxes under agitation condition, 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, centrifugation 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 (9)
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 comprising the steps:
(1) with ammonium persulphate-H
2SO
4Micro-etched waste liquid and basic solution are preheating to 50 ~ 100 ℃ respectively, and the micro-etched waste liquid that preheating is good joins in the neutralization reaction still that has whipping appts, when its add-on finishes for reaction 20% ~ 80% of the material cumulative volume;
(2) progressively add basic solution under agitation condition in above-mentioned micro-etched waste liquid and carry out neutralization reaction, the pH value scope in the control neutralization reaction still is between 8.0 ~ 13.0;
(3) add dispersion agent behind the filtering precipitate;
(4) filtrate of the above-mentioned pH of mixing up value is changed over to the ammonia still process reactor and carry out air distillation ammonia is therefrom overflowed, reduce to 7.5 ~ 8.5, finish ammonia still process to the pH value;
(5) with the Basic Chrome Sulphate in above-mentioned material precipitation more after filtration, washing, dry, obtain crystal type Basic Chrome Sulphate product after sieving.
2. the PCB ammonium persulphate-H that utilizes as claimed in claim 1
2SO
4Micro-etched waste liquid is produced the method for Basic Chrome Sulphate, it is characterized in that described ammonium persulphate-H
2SO
4Directly preheating in reactor of micro-etched waste liquid.
3. the PCB ammonium persulphate-H that utilizes as claimed in claim 1
2SO
4Micro-etched waste liquid is produced the method for Basic Chrome Sulphate, it is characterized in that described basic solution is one or more the mixture in NaOH, KOH, ammoniacal liquor, the slaked lime.
4. described in claim 1, utilize PCB ammonium persulphate-H
2SO
4Micro-etched waste liquid is produced the method for Basic Chrome Sulphate, it is characterized in that the pH value in step (2) or step (4) in employing pH electrode The real time measure neutralization reaction still, the ammonia still process reactor and the add-on and the ammonia still process time of control basic solution.
5. described in claim 1, utilize PCB ammonium persulphate-H
2SO
4Micro-etched waste liquid is produced the method for Basic Chrome Sulphate, it is characterized in that, dispersion agent described in the step (3) is one or more in the formaldehyde condensation products of Sodium dodecylbenzene sulfonate, sodium lignosulfonate, hydrolytic polymaleic anhydride, methyl naphthalene sulfonic acid sodium, and its weight is 2% ~ 8% of masterbatch.
6. described in claim 1, utilize PCB ammonium persulphate-H
2SO
4Micro-etched waste liquid is produced the method for Basic Chrome Sulphate, it is characterized in that the drying temperature in the step (5) is 40 ~ 80 ℃.
7. described in claim 1, utilize PCB ammonium persulphate-H
2SO
4Micro-etched waste liquid is produced the method for Basic Chrome Sulphate, it is characterized in that the ammonia still process temperature in the step (4) is 60 ~ 100 ℃, and the ammonia still process time is 0.5 ~ 3.5h.
8. described in claim 1, utilize PCB ammonium persulphate-H
2SO
4Micro-etched waste liquid is produced the method for Basic Chrome Sulphate, it is characterized in that, adopts water or excessive dilute sulphuric acid to absorb the ammonia that steams in the step (4).
9. described in claim 1, utilize PCB ammonium persulphate-H
2SO
4Micro-etched waste liquid is produced the method for Basic Chrome Sulphate, it is characterized in that described ammonium persulphate-H
2SO
4Copper concentration is 10 ~ 50g/L in the micro-etched waste liquid.
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 |
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| Publication Number | Publication Date |
|---|---|
| CN101780972A true CN101780972A (en) | 2010-07-21 |
| CN101780972B CN101780972B (en) | 2012-02-29 |
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|---|---|---|---|
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102815740A (en) * | 2012-08-03 | 2012-12-12 | 西北矿冶研究院 | Production method for improving copper sulfate grade |
| CN103435092A (en) * | 2013-09-01 | 2013-12-11 | 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) |
| CN103449501A (en) * | 2013-09-01 | 2013-12-18 | 深圳市危险废物处理站有限公司 | Comprehensive utilization method of waste liquor in production of basic cupric carbonate |
| 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 |
-
2010
- 2010-02-23 CN CN2010101171199A patent/CN101780972B/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102815740A (en) * | 2012-08-03 | 2012-12-12 | 西北矿冶研究院 | Production method for improving copper sulfate grade |
| CN102815740B (en) * | 2012-08-03 | 2015-04-22 | 西北矿冶研究院 | Production method for improving copper sulfate grade |
| CN103435092A (en) * | 2013-09-01 | 2013-12-11 | 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) |
| CN103449501A (en) * | 2013-09-01 | 2013-12-18 | 深圳市危险废物处理站有限公司 | Comprehensive utilization method of waste liquor in production of basic cupric carbonate |
| 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 |
| 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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