CN103991893A - Preparing method of high-purity basic cupric carbonate - Google Patents
Preparing method of high-purity basic cupric carbonate Download PDFInfo
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- CN103991893A CN103991893A CN201410200285.3A CN201410200285A CN103991893A CN 103991893 A CN103991893 A CN 103991893A CN 201410200285 A CN201410200285 A CN 201410200285A CN 103991893 A CN103991893 A CN 103991893A
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- Prior art keywords
- copper
- preparation
- ventilation breather
- ammonia
- air
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- 238000000034 method Methods 0.000 title abstract description 8
- ZMMDPCMYTCRWFF-UHFFFAOYSA-J dicopper;carbonate;dihydroxide Chemical compound [OH-].[OH-].[Cu+2].[Cu+2].[O-]C([O-])=O ZMMDPCMYTCRWFF-UHFFFAOYSA-J 0.000 title abstract 3
- 239000010949 copper Substances 0.000 claims abstract description 53
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 50
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 46
- 229910052802 copper Inorganic materials 0.000 claims abstract description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000001914 filtration Methods 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims abstract description 9
- 238000002386 leaching Methods 0.000 claims abstract description 9
- 238000001149 thermolysis Methods 0.000 claims abstract description 9
- 230000003647 oxidation Effects 0.000 claims abstract description 6
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 38
- 238000009423 ventilation Methods 0.000 claims description 38
- 238000002360 preparation method Methods 0.000 claims description 26
- 238000006243 chemical reaction Methods 0.000 claims description 19
- 229910021529 ammonia Inorganic materials 0.000 claims description 17
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 12
- 238000010521 absorption reaction Methods 0.000 claims description 12
- 238000000354 decomposition reaction Methods 0.000 claims description 9
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 8
- 235000011089 carbon dioxide Nutrition 0.000 claims description 8
- 239000003153 chemical reaction reagent Substances 0.000 claims description 8
- 238000009833 condensation Methods 0.000 claims description 8
- 230000005494 condensation Effects 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 239000000047 product Substances 0.000 claims description 8
- 239000004744 fabric Substances 0.000 claims description 6
- 239000012452 mother liquor Substances 0.000 claims description 6
- 238000012856 packing Methods 0.000 claims description 6
- 239000002244 precipitate Substances 0.000 claims description 6
- 238000012360 testing method Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 238000005422 blasting Methods 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 241000370738 Chlorion Species 0.000 claims description 3
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 3
- 238000002485 combustion reaction Methods 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 239000011889 copper foil Substances 0.000 claims description 3
- 229910001431 copper ion Inorganic materials 0.000 claims description 3
- GEZOTWYUIKXWOA-UHFFFAOYSA-L copper;carbonate Chemical compound [Cu+2].[O-]C([O-])=O GEZOTWYUIKXWOA-UHFFFAOYSA-L 0.000 claims description 3
- 238000005336 cracking Methods 0.000 claims description 3
- 238000013461 design Methods 0.000 claims description 3
- 238000007323 disproportionation reaction Methods 0.000 claims description 3
- 238000010298 pulverizing process Methods 0.000 claims description 3
- 238000000197 pyrolysis Methods 0.000 claims description 3
- 238000011084 recovery Methods 0.000 claims description 3
- 238000007873 sieving Methods 0.000 claims description 3
- 229910021653 sulphate ion Inorganic materials 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 239000006227 byproduct Substances 0.000 abstract description 5
- 239000002699 waste material Substances 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract 2
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 abstract 1
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 abstract 1
- 239000001099 ammonium carbonate Substances 0.000 abstract 1
- 238000003556 assay Methods 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 238000004806 packaging method and process Methods 0.000 abstract 1
- 230000002194 synthesizing effect Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 8
- 239000000460 chlorine Substances 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 3
- -1 generates Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 229910000365 copper sulfate Inorganic materials 0.000 description 1
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 229960003280 cupric chloride Drugs 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
Landscapes
- Electrolytic Production Of Metals (AREA)
- Treating Waste Gases (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a preparing method of high-purity basic cupric carbonate. Electrolytic copper, aqueous ammonia and ammonium bicarbonate are adopted as raw materials. The high-purity basic cupric carbonate is obtained by steps of preparing the aqueous ammonia, leaching and synthesizing, filtering, performing thermolysis, centrifuging to remove water, rinsing, drying, smashing, packaging after the assay is approved, and the like, and by adoption of secondary oxidation. The preparing method has characteristics of no production of side products, no production of waste materials, high utilization rate of the raw materials, low cost and no pollution.
Description
Technical field
The present invention relates to technical field of chemistry and chemical engineering, be specifically related to a kind of preparation method of high-purity ventilation breather.
Background technology
Ventilation breather belongs to field of fine chemical, is mainly used in organic catalyst, sterilant, electronic ceramics, crude oil storage dealkalize agent etc.The synthetic method of traditional ventilation breather is mainly to synthesize and generate ventilation breather with sodium carbonate or sodium hydrogen carbonate solution under dissolved state with copper sulfate, cupric chloride or cupric nitrate.This technique is because be synthetic under solution state, so solution body accumulated amount is large, because synthetic, need to be heated to comparatively high temps, so energy expenditure is large, the wastewater flow rate producing is large, in synthetic, produce the concentration of byproduct sodium chloride in the aqueous solution higher, thus be difficult for the sodium-chlor in product to clean separation, and the usage quantity of rinse water is also very large, the fineness of product is uncontrollable, the purity of product cannot reach market demand, therefore this process costs is high, wastewater flow rate is large, pollute heavy, yield poorly, energy consumption is large, and quality product is wayward.Therefore the preparation method who finds a kind of ventilation breather more cheaply more meets the development trend in market.
Summary of the invention
The object of the invention is to provide a kind of preparation method of high-purity ventilation breather, without byproduct and waste material, generates, and raw material availability is high, and cost is low, pollution-free.
For achieving the above object, the technical solution used in the present invention is: a kind of preparation method of high-purity ventilation breather, comprises the steps:
(1) prepare ammoniacal liquor: liquefied ammonia being passed under 0.2MPa pressure to deionized water and liquefied ammonia, to prepare concentration be 10%～12% ammoniacal liquor, stores for future use;
(2) leaching building-up reactions: in strip electrolytic copper packing into the copper pond of purity>=99.9%, pump into the ammoniacal liquor that makes in step (1) to flooding electrolytic copper, then by bicarbonate of ammonia/ammoniacal liquor mol ratio>=2, to changing in copper pond, add bicarbonate of ammonia, and from Hua Tongchi bottom, blasting air with air compressor machine, the air pressure in making copper pond is 1.01 * 10
5～10
6pa, controls 60 ℃～70 ℃ of temperature of reaction, to reacting, meets sulfuric acid test;
(3) filter: after 3/4 Schweitzeros reagent step (2) middleization copper pond in being drawn into the interior coarse filtration of strainer with pump, introduce the smart filtration of accurate filter, finally with pump, squeeze in reactor;
(4) thermolysis: utilize air compressor machine to blast air in reactor, and will in reactor, be warming up to 80～100 ℃, carry out secondary oxidation and air lift, remove through the unsegregated micro-copper powder of twice filtration, also make cuprammonium compound generation decomposition reaction generate ventilation breather simultaneously, detect in the mixed liquor that contains ventilation breather after its decomposition reaction when copper ion concentration is less than 10g/L, decomposition reaction finishes; And the thermolysis water vapour that contains ammonia and carbonic acid gas out enters condenser with air, it is stand-by that the carbonated aqueous ammonia generating during condensation is sent into strong aqua preparation vessel;
(5) water dumping, rinsing: the mixed liquor that contains ventilation breather that pyrolysis is obtained is squeezed into whizzer, first get rid of mother liquor to the greatest extent wherein, then with deionized water wash, finish washing during to chlorion mass concentration≤20ppm in washing water, from whizzer, hang out the ventilation breather that contains a small amount of moisture content;
(6) dry, pulverize: it is to be dried to the rear pulverizing of moisture≤2% in the baking oven of 50～70 ℃ that the ventilation breather that contains a small amount of moisture in step (5) is delivered to design temperature, and after sieving by 100 orders, pulverize, packing, both basic carbonate copper products.
Wherein, in described step (1), the ammoniacal liquor of preparation is stored in reservoir standby.
Wherein, in described step (2), with sheet shears, electrolytic copper foil is cut into strip;
In described step (2), before being pumped to of ammoniacal liquor copper pond, through cloth envelop collector, filter.
Wherein, in described step (2), the chemical equation of leaching building-up reactions is:
2Cu+2NH
4HCO
3+2NH
3+O
2=2Cu(NH
3)
2CO
3+2H
2O。
Wherein, in described step (2), sulfuric acid test is: add sulphate reagent in 3～5ml reaction solution after, do not produce red precipitate, detect according to being:
Cu (NH
3)
2cO
3+ H
2sO
4→ CuSO
4blue look solution, illustrates completely reacted;
Cu (OH)
2cO
3+ H
2sO
4→ CuSO
4+ Cu ↓ red precipitate is copper powder, illustrates that unreacted is good.
Wherein, in described step (4), cracking chemical reaction formula is:
3Cu(NH
3)
2CO
3+H
2O=2CuCO
3·Cu(OH)
2↓+6NH
3↑+CO
2↑。
Wherein, in described step (4), the concrete reaction that the thermolysis water vapour that contains ammonia and carbonic acid gas out enters after condenser with air is: during condensation, part ammonia and carbonic acid gas enter phlegma and generate carbonated aqueous ammonia, carbonated aqueous ammonia is squeezed into the residual air that absorption tower absorption condensation is come after cooling, it is stand-by that carbonated aqueous ammonia after absorption residual air is sent strong aqua preparation vessel back to, after in the inner exhaust gas of absorption tower, the ammonia of trace is sent into boiler combustion with gas blower, discharges.
Wherein, in described step (5), the rinse water that when hanging out ventilation breather from whizzer, the mother liquor that just starts to throw away and first three time thrown away merge in adding copper pond the raw material when next timeization copper reacts, and finally rinse water are delivered to carbonated aqueous ammonia recovery tower for the preparation of ammoniacal liquor several times.
Wherein, in described step (3), Schweitzeros reagent is carried out to the strainer of coarse filtration and select cloth envelop collector, change residual copper ammoniacal liquor in copper pond and make lower batch disproportionation reaction with accelerationization copper speed.
Wherein, in described step (4), with air compressor machine, when blasting air in reactor, outlet air temperature is 40 ℃～50 ℃, and the pressure of air compressor machine is 6～8kg.
Because technique scheme is used, the present invention compared with prior art has following advantages:
It is raw material that electrolytic copper, ammoniacal liquor, bicarbonate of ammonia are take in the present invention, and by leaching building-up reactions, whole process adopts deionized water, and take secondary oxidation to reach high-purity, low chlorine ventilation breather, and without byproduct and waste material, generating, raw material availability is high, cost is low, pollution-free.
Embodiment
Below in conjunction with embodiment, the invention will be further described:
Embodiment mono-: a kind of preparation method of high-purity ventilation breather, comprises the steps:
(1) prepare ammoniacal liquor: liquefied ammonia being passed under 0.2MPa pressure to deionized water and liquefied ammonia, to prepare concentration be 10%～12% ammoniacal liquor, is stored in reservoir standby;
(2) leaching building-up reactions: the electrolytic copper foil of purity>=99.9% is cut in strip electrolytic copper packing into copper pond with sheet shears, by the ammoniacal liquor making in step (1) after cloth envelop collector filters in pumping into copper pond to flooding electrolytic copper, then by bicarbonate of ammonia/ammoniacal liquor mol ratio>=2, to changing in copper pond, add bicarbonate of ammonia, and from Hua Tongchi bottom, blast air, the air pressure 1.01 * 10 in making copper pond with air compressor machine
5～10
6pa, controls 60 ℃～70 ℃ of temperature of reaction, to reacting, meets sulfuric acid test, and the chemical equation of described leaching building-up reactions is:
2Cu+2NH
4HCO
3+2NH
3+O
2=2Cu(NH
3)
2CO
3+2H
2O；
Wherein, described sulfuric acid test is: add sulphate reagent in 3～5ml reaction solution after, do not produce red precipitate, detect according to being:
Cu (NH
3)
2cO
3+ H
2sO
4→ CuSO
4blue look solution, illustrates completely reacted;
Cu (OH)
2cO
3+ H
2sO
4→ CuSO
4+ Cu ↓ red precipitate is copper powder, illustrates that unreacted is good.
(3) filter: after 3/4 Schweitzeros reagent step (2) middleization copper pond in being drawn into the interior coarse filtration of cloth envelop collector with pump, introduce the smart filtration of accurate filter, finally with pump, squeeze in reactor, change residual copper ammoniacal liquor in copper pond and make lower batch disproportionation reaction with accelerationization copper speed.
(4) thermolysis: (outlet air temperature is 40 ℃～50 ℃ to utilize air compressor machine, the pressure of air compressor machine is 6～8kg) in reactor, blast air, and will in reactor, be warming up to 80～100 ℃, carry out secondary oxidation and air lift, remove through the unsegregated micro-copper powder of twice filtration, also make cuprammonium compound generation decomposition reaction generate ventilation breather simultaneously, detect in the mixed liquor that contains ventilation breather after its decomposition reaction when copper ion concentration is less than 10g/L, decomposition reaction finishes; And the thermolysis water vapour that contains ammonia and carbonic acid gas out enters condenser with air, during condensation, part ammonia and carbonic acid gas enter phlegma and generate carbonated aqueous ammonia, carbonated aqueous ammonia is squeezed into the residual air that absorption tower absorption condensation is come after cooling, it is stand-by that carbonated aqueous ammonia after absorption residual air is sent strong aqua preparation vessel back to, after in the inner exhaust gas of absorption tower, the ammonia of trace is sent into boiler combustion with gas blower, discharge, cracking chemical reaction formula is:
3Cu(NH
3)
2CO
3+H
2O=2CuCO
3·Cu(OH)
2↓+6NH
3↑+CO
2↑。
(5) water dumping, rinsing: the mixed liquor that contains ventilation breather that pyrolysis is obtained is squeezed into whizzer, first get rid of mother liquor to the greatest extent wherein, then with deionized water wash, finish washing during to chlorion mass concentration≤20ppm in washing water, from whizzer, hang out the ventilation breather that contains a small amount of moisture content; The rinse water that simultaneously mother liquor that just starts to throw away and first three time thrown away merge in adding copper pond the raw material when next timeization copper reacts, and finally rinse water are delivered to carbonated aqueous ammonia recovery tower for the preparation of ammoniacal liquor several times.
(6) dry, pulverize: it is to be dried to the rear pulverizing of moisture≤2% in the baking oven of 50～70 ℃ that the ventilation breather that contains a small amount of moisture in step (5) is delivered to design temperature, and after sieving by 100 orders, pulverize, packing, both basic carbonate copper products.
The technical indicator that obtains product is as following table:
| Index subjet | Business indicators | Prior art index | Index of the present invention |
| Copper (Cu) % >= | 55 | 50 | 55.6 |
| Plumbous (Pb) %≤ | 20 | 30 | 7.5 |
| Chlorine (Cl) ppm≤ | 100 | 700 | 50 |
| Calcium (Ca) ppm≤ | 50 | 300 | 10 |
| Chromium (Cr) ppm≤ | 10 | 30 | ND |
| Sodium (Na) ppm≤ | 150 | 2500 | 80 |
| Arsenic (As) ppm≤ | 10 | 50 | 12 |
| Iron (Fe) ppm≤ | 50 | 300 | 120.5 |
| Cadmium (Cd) ppm≤ | 5 | 6 | 0.5 |
| Vitriol ppm≤ | 150 | 700 | 150 |
| Hydrochloric acid insoluble substance %≤ | 0.05 | 0.1 | 0.006 |
| Moisture %≤ | 2.0 | 1 | 0.02 |
It is raw material that electrolytic copper, ammoniacal liquor, bicarbonate of ammonia are take in the present invention, and by leaching building-up reactions, whole process adopts deionized water, and take secondary oxidation to reach high-purity, low chlorine ventilation breather, and without byproduct and waste material, generating, raw material availability is high, cost is low, pollution-free.
The above is the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, do not departing under the prerequisite of principle of the present invention; can also make some improvement or replacement, these improvement or replacement also should be considered as protection scope of the present invention.
Claims (10)
1. a preparation method for high-purity ventilation breather, is characterized in that, comprises the steps:
(1) prepare ammoniacal liquor: liquefied ammonia being passed under 0.2MPa pressure to deionized water and liquefied ammonia, to prepare concentration be 10%～12% ammoniacal liquor, stores for future use;
(2) leaching building-up reactions: in strip electrolytic copper packing into the copper pond of purity>=99.9%, pump into the ammoniacal liquor that makes in step (1) to flooding electrolytic copper, then by bicarbonate of ammonia/ammoniacal liquor mol ratio>=2, to changing in copper pond, add bicarbonate of ammonia, and from Hua Tongchi bottom, blasting air with air compressor machine, the air pressure in making copper pond is 1.01 * 10
5～10
6pa, controls 60 ℃～70 ℃ of temperature of reaction, to reacting, meets sulfuric acid test;
(3) filter: after 3/4 Schweitzeros reagent step (2) middleization copper pond in being drawn into the interior coarse filtration of strainer with pump, introduce the smart filtration of accurate filter, finally with pump, squeeze in reactor;
(4) thermolysis: utilize air compressor machine to blast air in reactor, and will in reactor, be warming up to 80～100 ℃, carry out secondary oxidation and air lift, remove through the unsegregated micro-copper powder of twice filtration, also make cuprammonium compound generation decomposition reaction generate ventilation breather simultaneously, detect in the mixed liquor that contains ventilation breather after its decomposition reaction when copper ion concentration is less than 10g/L, decomposition reaction finishes; And the thermolysis water vapour that contains ammonia and carbonic acid gas out enters condenser with air, it is stand-by that the carbonated aqueous ammonia generating during condensation is sent into strong aqua preparation vessel;
(5) water dumping, rinsing: the mixed liquor that contains ventilation breather that pyrolysis is obtained is squeezed into whizzer, first get rid of mother liquor to the greatest extent wherein, then with deionized water wash, finish washing during to chlorion mass concentration≤20ppm in washing water, from whizzer, hang out the ventilation breather that contains a small amount of moisture content;
(6) dry, pulverize: it is to be dried to the rear pulverizing of moisture≤2% in the baking oven of 50～70 ℃ that the ventilation breather that contains a small amount of moisture in step (5) is delivered to design temperature, and after sieving by 100 orders, pulverize, packing, both basic carbonate copper products.
2. the preparation method of high-purity ventilation breather according to claim 1, is characterized in that, in described step (1), the ammoniacal liquor of preparation is stored in reservoir standby.
3. the preparation method of high-purity ventilation breather according to claim 1, is characterized in that, in described step (2), with sheet shears, electrolytic copper foil is cut into strip;
In described step (2), before being pumped to of ammoniacal liquor copper pond, through cloth envelop collector, filter.
4. the preparation method of high-purity ventilation breather according to claim 1, is characterized in that, in described step (2), the chemical equation of leaching building-up reactions is:
2Cu+2NH
4HCO
3+2NH
3+O
2=2Cu(NH
3)
2CO
3+2H
2O。
5. the preparation method of high-purity ventilation breather according to claim 1, is characterized in that, in described step (2), sulfuric acid test is: add sulphate reagent in 3～5ml reaction solution after, do not produce red precipitate, detect according to being:
Cu (NH
3)
2cO
3+ H
2sO
4→ CuSO
4blue look solution, illustrates completely reacted;
Cu (OH)
2cO
3+ H
2sO
4→ CuSO
4+ Cu ↓ red precipitate is copper powder, illustrates that unreacted is good.
6. the preparation method of high-purity ventilation breather according to claim 1, is characterized in that, in described step (4), cracking chemical reaction formula is:
3Cu(NH
3)
2CO
3+H
2O=2CuCO
3·Cu(OH)
2↓+6NH
3↑+CO
2↑。
7. the preparation method of high-purity ventilation breather according to claim 1, it is characterized in that, in described step (4), the concrete reaction that the thermolysis water vapour that contains ammonia and carbonic acid gas out enters after condenser with air is: during condensation, part ammonia and carbonic acid gas enter phlegma and generate carbonated aqueous ammonia, carbonated aqueous ammonia is squeezed into the residual air that absorption tower absorption condensation is come after cooling, it is stand-by that carbonated aqueous ammonia after absorption residual air is sent strong aqua preparation vessel back to, after in the inner exhaust gas of absorption tower, the ammonia of trace is sent into boiler combustion with gas blower, discharges.
8. the preparation method of high-purity ventilation breather according to claim 1, it is characterized in that, in described step (5), the rinse water that when hanging out ventilation breather from whizzer, the mother liquor that just starts to throw away and first three time thrown away merge in adding copper pond the raw material when next timeization copper reacts, and finally rinse water are delivered to carbonated aqueous ammonia recovery tower for the preparation of ammoniacal liquor several times.
9. the preparation method of high-purity ventilation breather according to claim 1, it is characterized in that, in described step (3), Schweitzeros reagent is carried out to the strainer of coarse filtration and select cloth envelop collector, change residual copper ammoniacal liquor in copper pond and make lower batch disproportionation reaction with accelerationization copper speed.
10. the preparation method of high-purity ventilation breather according to claim 1, is characterized in that, in described step (4), with air compressor machine, when blasting air in reactor, outlet air temperature is 40 ℃～50 ℃, and the pressure of air compressor machine is 6～8kg.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105753049A (en) * | 2016-01-26 | 2016-07-13 | 苏州优合科技有限公司 | Preparation method of basic copper carbonate |
| CN106395882A (en) * | 2016-12-06 | 2017-02-15 | 杜宗鑫 | Device and process using ammonia method to produce metal compounds |
| CN107324373A (en) * | 2017-07-18 | 2017-11-07 | 清华大学 | The method of purification of malachite pigment |
| CN115028186A (en) * | 2022-05-05 | 2022-09-09 | 金川集团股份有限公司 | Process for producing copper compound by using alkali leaching copper dissolving method |
| CN115029561A (en) * | 2022-05-05 | 2022-09-09 | 金川集团股份有限公司 | Leaching process for preparing high-purity alkaline copper-containing solution |
| CN116477655A (en) * | 2023-06-14 | 2023-07-25 | 泰兴冶炼厂有限公司 | A method for continuous production of light high-purity basic copper carbonate |
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2014
- 2014-05-14 CN CN201410200285.3A patent/CN103991893A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105753049A (en) * | 2016-01-26 | 2016-07-13 | 苏州优合科技有限公司 | Preparation method of basic copper carbonate |
| CN106395882A (en) * | 2016-12-06 | 2017-02-15 | 杜宗鑫 | Device and process using ammonia method to produce metal compounds |
| TWI636015B (en) * | 2016-12-06 | 2018-09-21 | 杜宗鑫 | Device for producing metal compound by ammonia method and production process thereof |
| CN107324373A (en) * | 2017-07-18 | 2017-11-07 | 清华大学 | The method of purification of malachite pigment |
| CN107324373B (en) * | 2017-07-18 | 2019-05-28 | 清华大学 | The method of purification of malachite pigment |
| CN115028186A (en) * | 2022-05-05 | 2022-09-09 | 金川集团股份有限公司 | Process for producing copper compound by using alkali leaching copper dissolving method |
| CN115029561A (en) * | 2022-05-05 | 2022-09-09 | 金川集团股份有限公司 | Leaching process for preparing high-purity alkaline copper-containing solution |
| CN116477655A (en) * | 2023-06-14 | 2023-07-25 | 泰兴冶炼厂有限公司 | A method for continuous production of light high-purity basic copper carbonate |
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