CN104120486B - Composite wire separation process and equipment thereof - Google Patents
Composite wire separation process and equipment thereof Download PDFInfo
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- CN104120486B CN104120486B CN201410374513.9A CN201410374513A CN104120486B CN 104120486 B CN104120486 B CN 104120486B CN 201410374513 A CN201410374513 A CN 201410374513A CN 104120486 B CN104120486 B CN 104120486B
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Abstract
The invention relates to a composite wire separation process and equipment thereof, wherein the process comprises the following steps: (a) separation: oxidizing and removing copper in the composite wire by using separation liquid containing ferric ions with the content of 40-50 g/L to obtain metal fibers, wherein the temperature of the separation liquid is 80-90 ℃, and the content of hydrogen ions in the separation liquid is 0.5-1 g/L; (b) and (3) oxidation: oxidizing ferrous ions in the separated liquid after the step (a) is finished into ferric ions by using an oxidizing agent; (c) and (3) extraction: extracting divalent copper ions in the separation liquid after the step (b) is finished into an organic phase and separating the organic phase from a water phase; (d) heating: the extracted water phase becomes separated liquid again after being heated. The equipment suitable for the above-mentioned line-closing separation process is formed from separation tank (1), oxidation tank (3), extraction box (4) and heating tank (2) which are successively unidirectionally connected, and formed into a circulation. The composite line separation process provided by the invention has continuous production and high separation speed; the separation effect is good, and the produced metal fiber is free from corrosion; no industrial pollution and environmental protection.
Description
Technical field
The present invention relates to a kind of recombination line separating technology and its equipment.
Background technology
Metallic fiber is produced in recent years because application field is constantly expanded in bundle drawing method method, and market demand increases year by year
Plus, the widely used metallic fiber in market is stainless steel fibre and iron-chromium-aluminum.Gold is being produced in bundle drawing method method
Belong to fiber technique in, first after metal wire material, isolated material, covering material boundling by multiple tube reducing drawing and annealing after system
Recombination line is produced, then metallic fiber will be manufactured after the isolated material in recombination line and covering material removal.Recombination line is continuously separated
Technique is the conventional process for producing high-quality metallic fiber, and existing recombination line continuous separation technology is all to use electrochemical electrolysis
Technique, the copper in recombination line is transferred to negative electrode by the method being electrolysed, so as to reach the purpose that the copper in recombination line is removed, should
Due to needing using recombination line as anode, electric current is needed to pass through from recombination line technique, and recombination line is contacted under mobile status
Formula is conductive, and high current can burn out conductive contact and recombination line, cause electrolytic current density low, so electrochemical electrolysis process yields
It is low.Recombination line in electrolytic process because metal wire material gradually scatters, it is conductive and uneven between metal wire material, and negative and positive
The pole span of pole is also uneven, and the near metal wire material of pole span is first electrolysed, so causing recombination line to be electrolysed uneven influence metallic fiber
Product quality.The anode of electrochemical electrolysis technique is recombination line in linear, the cathode copper on minus plate can be formed copper post or
Copper knurl, if cleaning can hang up recombination line, it is necessary to often shut down cleaning copper post and copper knurl not in time, so as to reduce metallic fiber product
Amount.The cathode copper outward appearance out-of-flatness of the production on minus plate, reduces the quality of cathode copper.Cathode copper production is to needing after a certain amount of
Taking-up cathode copper is shut down, the yield of metallic fiber can be also reduced.
The content of the invention
Present invention aim to address the yielding poorly of the metallic fiber in above-mentioned recombination line separating technology, of poor quality and production
Continuity problem not high.
To achieve the above object, the present invention uses a kind of recombination line separating technology, comprises the following steps：A () separates：Use
Metallic fiber is obtained for the separation liquid oxidation of the ferric ion of 40-50 g/L removes the copper in recombination line containing content, is separated
The temperature of liquid is 80-90 DEG C, and hydrionic content is 0.5-1 g/L in separating liquid；B () aoxidizes：Using oxidant by step
A the oxidation of divalent iron ion in separating liquid after the completion of () is into ferric ion；C () extracts：By the separation after the completion of step (b)
Bivalent cupric ion is extracted into organic phase and separated from the water in liquid；D () heats：Turn into again after water after extraction is mutually heated point
Chaotropic.
Further, the organic phase after the extraction obtains copper by back extraction, electrodeposition again.
Further, the balance anion preferably sulfuric acid radical ion in the separating liquid.
Further, in the separating liquid ferrous ion content be 1-10 g/L, bivalent cupric ion content be 1-15 g/
L。
Further, the oxidant in the step (b) is hydrogen peroxide, ozone, pure oxygen, air, preferably hydrogen peroxide.
The present invention also provide it is a kind of be adapted to above-mentioned recombination line separating technology equipment, by separating tank, oxidation trough, extraction box and
Heating tank is constituted, and separating tank, oxidation trough, extraction box and heating tank are unidirectionally connected and form circulation successively.
Further, back extraction case and Winning cell are connected on the extraction box of the said equipment, wherein back extraction case and extraction box, electricity
Product groove is and is bi-directionally connected and is respectively formed circulation.
Ferric ion in the separating liquid makes the copper in recombination line be oxidized to bivalent cupric ion, while ferric ion
Ferrous ion is reduced into, with hydrogen peroxide oxidation of divalent iron ion into ferric ion in oxidation trough, and in extraction box
Using bivalent cupric ion is isolated in extractant, the solution of ferric ion comes back to separating tank by heating tank heating to be turned into
Separating liquid.
After extraction, bivalent cupric ion is present in the organic phase of extraction box；The acid of high concentration, extraction are run into case is stripped
Take agent and recombine regeneration with hydrogen, reenter extraction box for extracting, bivalent cupric ion flows into electrodeposition in reentering water phase
Groove；In Winning cell electrolytic deposition copper, while producing oxygen and hydrogen ion, hydrogen ion enters back into back extraction case to be used to be stripped.
Described being separated into is continuously separated, and the extraction of bivalent cupric ion is not in the oxidation reaction and extraction box in oxidation trough
Can carry out thoroughly, therefore also contain ferrous ion in separating liquid：1-10 g/L, bivalent cupric ion：1-15 g/L.
Isolated material, covering material in the technique of bundle drawing method method production metallic fiber usually select copper, are oxidation
Copper is removed, the oxidation resistance of metal wire material need to be stronger than copper in recombination line, conventional material is stainless steel and ferrum-chromium-aluminum.
The beneficial effects of the present invention are：The production of recombination line separating technology is continuous, and separating rate is fast；Good separating effect, it is raw
The metallic fiber of product is corrosion-free；Without industrial pollution, environmental protection.The production solved in Electrochemical separation technique is discontinuous, raw
Product yields poorly, it is necessary to shut down cleaning cathode copper, the problems such as part metals fiber electrolytic etching.
Brief description of the drawings
Fig. 1：Implement the schematic device of present invention process.
In figure：1st, separating tank, 2, heating tank, 3, oxidation trough, 4, extraction box, 5, back extraction case, 6, Winning cell, 7, recombination line,
8th, metallic fiber.
Specific embodiment
Below in conjunction with the accompanying drawings, comparative example and embodiment illustrate the features of the present invention and technique effect, but the present invention is not limited
In specific embodiment.Extractant described in embodiment is peaceful (Cognis) company copper extractant Lix984N of Dutch section；Embodiment with
The size of separating tank described in comparative example only length is different, and the number of recombination line is 24 in separating tank.
Comparative example：
Copper is separated off using electrochemical electrolysis, the m of flute length 120, the g/L of hydrogen ion content 0.5, divalence in electrolyte is separated
The g/L of 12 g/L bivalent cupric ions content of iron ion content 13, balance anion is sulfate ion；The V of DC electrolysis voltage 2.
Recombination line enters separating tank by the speed of 0.65 m/min, average daily output metallic fiber 60 kg.
Embodiment 1：
Separating tank 1 grow 55 m, the starting soln of separating tank 1 be ferric sulfate and sulfuric acid, the g/L of ferric ion content 50, hydrogen from
The g/L of sub- content 1,85 DEG C of separating liquid temperature, recombination line 7 enters separating tank 1 by the speed of 1.04 m/min, in recombination line 7
Copper generates copper sulphate and ferrous sulfate with the ferric sulfate reaction in separating liquid, and all removal just turns into metal to the copper in recombination line 7
Fiber 8.The separating liquid of separating tank 1 enters oxidation trough 3, and solution composition is ferric sulfate, ferrous sulfate, copper sulphate, sulfuric acid, uses dioxygen
Ferrous sulfate is oxidized to ferric sulfate by water, and the solution after oxidation enters extraction box 4.Extractant in extraction box 4 and cupric from
Son is combined, and the bivalent cupric ion of organic phase is separated from the water；Water back flows back into separating tank 1 after being heated into heating tank 2 to be turned into
Separating liquid, the bivalent cupric ion in organic phase enters back extraction case 5.Bivalent cupric ion back extraction is entered water by the sulfuric acid in back extraction case 5
Mutually turn into copper-bath and enter Winning cell 6, while the extractant regeneration of organic phase reenters extraction box 4.Copper-bath
Copper, oxygen and sulfuric acid are obtained into the electrolytic deposition of Winning cell 6, sulfuric acid comes back to back extraction case 5 to be used to be stripped.Whole technique is continuous
Operation, stabilization after separating tank 1 separating liquid composition be the g/L of ferric ion content 47, the g/L of ferrous ion content 3, copper from
The g/L of sub- content 4, the g/L of hydrogen ion content 1,85 DEG C of separating liquid temperature, average daily output metallic fiber 100 kg.
Embodiment 2：
Separating tank 1 grow 55 m, the starting soln of separating tank 1 be ferric sulfate and sulfuric acid, the g/L of ferric ion content 42, hydrogen from
The g/L of sub- content 1,80 DEG C of separating liquid temperature, recombination line 7 enters separating tank 1 by the speed of 1.15 m/min, in recombination line 7
Copper generates copper sulphate and ferrous sulfate with the ferric sulfate reaction in separating liquid, and all removal just turns into metal to the copper in recombination line 7
Fiber 8.The separating liquid of separating tank 1 enters oxidation trough 3, and solution composition is ferric sulfate, ferrous sulfate, copper sulphate, sulfuric acid, uses dioxygen
Ferrous sulfate is oxidized to ferric sulfate by water, and the solution after oxidation enters extraction box 4.Extractant in extraction box 4 and cupric from
Son is combined, and the bivalent cupric ion of organic phase is separated from the water；Water back flows back into separating tank 1 after being heated into heating tank 2 to be turned into
Separating liquid, the bivalent cupric ion in organic phase enters back extraction case 5.Bivalent cupric ion back extraction is entered water by the sulfuric acid in back extraction case 5
Mutually turn into copper-bath and enter Winning cell 6, while the extractant regeneration of organic phase reenters extraction box 4.Copper-bath
Copper, oxygen and sulfuric acid are obtained into the electrolytic deposition of Winning cell 6, sulfuric acid comes back to back extraction case 5 to be used to be stripped.Whole technique is continuous
Operation, the separating liquid composition of separating tank 1 is the g/L of ferric ion content 40, the g/L of ferrous ion content 10, copper after stabilization
The g/L of ion concentration 10, the g/L of hydrogen ion content 1,80 DEG C of separating liquid temperature, average daily output metallic fiber 80 kg.
Embodiment 3：
Separating tank 1 grow 55 m, the starting soln of separating tank 1 be ferric sulfate and sulfuric acid, the g/L of ferric ion content 50, hydrogen from
The g/L of sub- content 1,85 DEG C of separating liquid temperature, recombination line 7 enters separating tank 1, the copper in recombination line 7 by the speed of 1.4 m/min
With ferric sulfate reaction generation copper sulphate and ferrous sulfate in separating liquid, all removal is fine with regard to turning into metal for the copper in recombination line 7
Dimension 8.The separating liquid of separating tank 1 enters oxidation trough 3, and solution composition is ferric sulfate, ferrous sulfate, copper sulphate, sulfuric acid, uses hydrogen peroxide
Ferrous sulfate is oxidized to ferric sulfate, the solution after oxidation enters extraction box 4.Extractant and bivalent cupric ion in extraction box 4
With reference to the bivalent cupric ion of organic phase is separated from the water；Water into heating tank 2 heat after back flow back into separating tank 1 turn into point
Chaotropic, the bivalent cupric ion in organic phase enters back extraction case 5.Bivalent cupric ion back extraction is entered water phase by the sulfuric acid in back extraction case 5
Enter Winning cell 6 as copper-bath, while the extractant regeneration of organic phase reenters extraction box 4.Copper-bath enters
Enter the electrolytic deposition of Winning cell 6 and obtain copper, oxygen and sulfuric acid, sulfuric acid comes back to back extraction case 5 to be used to be stripped.Whole technique is continuously transported
OK, stabilization after separating tank 1 separating liquid composition be the g/L of ferric ion content 44, the g/L of ferrous ion content 11, copper from
The g/L of sub- content 15, the g/L of hydrogen ion content 1,85 DEG C of separating liquid temperature, average daily output metallic fiber 135 kg.
Embodiment 4：
Separating tank 1 grow 55 m, the starting soln of separating tank 1 be ferric sulfate and sulfuric acid, the g/L of ferric ion content 45, hydrogen from
The g/L of sub- content 0.5,80 DEG C of separating liquid temperature, recombination line 7 enters separating tank 1 by the speed of 1.3 m/min, in recombination line 7
Copper generates copper sulphate and ferrous sulfate with the ferric sulfate reaction in separating liquid, and all removal just turns into metal to the copper in recombination line 7
Fiber 8.The separating liquid of separating tank 1 enters oxidation trough 3, and solution composition is ferric sulfate, ferrous sulfate, copper sulphate, sulfuric acid, uses dioxygen
Ferrous sulfate is oxidized to ferric sulfate by water, and the solution after oxidation enters extraction box 4.Extractant in extraction box 4 and cupric from
Son is combined, and the bivalent cupric ion of organic phase is separated from the water；Water back flows back into separating tank 1 after being heated into heating tank 2 to be turned into
Separating liquid, the bivalent cupric ion in organic phase enters back extraction case 5.Bivalent cupric ion back extraction is entered water by the sulfuric acid in back extraction case 5
Mutually turn into copper-bath and enter Winning cell 6, while the extractant regeneration of organic phase reenters extraction box 4.Copper-bath
Copper, oxygen and sulfuric acid are obtained into the electrolytic deposition of Winning cell 6, sulfuric acid comes back to back extraction case 5 to be used to be stripped.Whole technique is continuous
Operation, stabilization after separating tank 1 separating liquid composition be the g/L of ferric ion content 42, the g/L of ferrous ion content 5, copper from
The g/L of sub- content 6, the g/L of hydrogen ion content 0.5,80 DEG C of separating liquid temperature, average daily output metallic fiber 125 kg.
Embodiment 5：
Separating tank 1 grow 55 m, the starting soln of separating tank 1 be ferric sulfate and sulfuric acid, the g/L of ferric ion content 48, hydrogen from
The g/L of sub- content 0.5,80 DEG C of separating liquid temperature, recombination line 7 enters separating tank 1 by the speed of 1.33 m/min, in recombination line 7
Copper and separating liquid in ferric sulfate reaction generation copper sulphate and ferrous sulfate, all removal just turns into gold to the copper in recombination line 7
Category fiber 8.The separating liquid of separating tank 1 enters oxidation trough 3, and solution composition is ferric sulfate, ferrous sulfate, copper sulphate, sulfuric acid, with double
Ferrous sulfate is oxidized to ferric sulfate by oxygen water, and the solution after oxidation enters extraction box 4.Extractant and cupric in extraction box 4
Ions binding, the bivalent cupric ion of organic phase is separated from the water；Water back flows back into 1 one-tenth of separating tank after being heated into heating tank 2
It is separating liquid, the bivalent cupric ion in organic phase enters back extraction case 5.Be stripped for bivalent cupric ion and enter by the sulfuric acid in back extraction case 5
Water mutually turns into copper-bath and enters Winning cell 6, while the extractant regeneration of organic phase reenters extraction box 4.Copper sulphate is molten
Liquid obtains copper, oxygen and sulfuric acid into the electrolytic deposition of Winning cell 6, and sulfuric acid comes back to back extraction case 5 to be used to be stripped.Whole technique connects
Reforwarding row, the separating liquid composition of separating tank 1 is the g/L of ferric ion content 46, the g/L of ferrous ion content 6, copper after stabilization
The g/L of ion concentration 7, the g/L of hydrogen ion content 0.5,80 DEG C of separating liquid temperature, average daily output metallic fiber 130 kg.
Embodiment 6：
Separating tank 1 grow 55 m, the starting soln of separating tank 1 be ferric sulfate and sulfuric acid, the g/L of ferric ion content 50, hydrogen from
The g/L of sub- content 0.5,90 DEG C of separating liquid temperature, recombination line 7 enters separating tank 1 by the speed of 2.08 m/min, in recombination line 7
Copper and separating liquid in ferric sulfate reaction generation copper sulphate and ferrous sulfate, all removal just turns into gold to the copper in recombination line 7
Category fiber 8.The separating liquid of separating tank 1 enters oxidation trough 3, and solution composition is ferric sulfate, ferrous sulfate, copper sulphate, sulfuric acid, with double
Ferrous sulfate is oxidized to ferric sulfate by oxygen water, and the solution after oxidation enters extraction box 4.Extractant and cupric in extraction box 4
Ions binding, the bivalent cupric ion of organic phase is separated from the water；Water back flows back into 1 one-tenth of separating tank after being heated into heating tank 2
It is separating liquid, the bivalent cupric ion in organic phase enters back extraction case 5.Be stripped for bivalent cupric ion and enter by the sulfuric acid in back extraction case 5
Water mutually turns into copper-bath and enters Winning cell 6, while the extractant regeneration of organic phase reenters extraction box 4.Copper sulphate is molten
Liquid obtains copper, oxygen and sulfuric acid into the electrolytic deposition of Winning cell 6, and sulfuric acid comes back to back extraction case 5 to be used to be stripped.Whole technique connects
Reforwarding row, the separating liquid composition of separating tank 1 is the g/L of ferric ion content 48, the g/L of ferrous ion 5, copper ion after stabilization
6 g/L, the g/L of hydrogen ion content 0.8,90 DEG C of separating liquid temperature, average daily output metallic fiber 185 kg.
Claims (5)
1. a kind of recombination line separating technology, it is characterised in that comprise the following steps：A () separates：The use of containing content is 40-50
The copper that the separation liquid oxidation of the ferric ion of g/L is removed in recombination line obtains metallic fiber, and the temperature of separating liquid is 80-90
DEG C, hydrionic content is 0.5-1 g/L in separating liquid, and the balance anion in the separating liquid is sulfate ion；(b) oxygen
Change：Using oxidant by the oxidation of divalent iron ion in the separating liquid after the completion of step (a) into ferric ion；C () extracts：Will
Bivalent cupric ion is extracted into organic phase and separated from the water in separating liquid after the completion of step (b)；D () heats：Water after extraction
Again separating liquid is turned into after mutually heated.
2. recombination line separating technology as claimed in claim 1, it is characterised in that organic phase after the extraction again by back extraction,
Electrodeposition obtains copper.
3. recombination line separating technology as claimed in claim 1 or 2, it is characterised in that ferrous ion content in the separating liquid
For 1-10 g/L, bivalent cupric ion content are 1-15 g/L.
4. recombination line separating technology as claimed in claim 1 or 2, it is characterised in that the oxidant in the step (b) is double
Oxygen water, ozone, pure oxygen or air.
5. recombination line separating technology as claimed in claim 4, it is characterised in that the oxidant in the step (b) is dioxygen
Water.
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| CN201410374513.9A CN104120486B (en) | 2014-08-01 | 2014-08-01 | Composite wire separation process and equipment thereof |
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| CN201410374513.9A CN104120486B (en) | 2014-08-01 | 2014-08-01 | Composite wire separation process and equipment thereof |
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| CN104120486A CN104120486A (en) | 2014-10-29 |
| CN104120486B true CN104120486B (en) | 2017-06-16 |
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| CN107513792A (en) * | 2017-07-07 | 2017-12-26 | 湖南汇博金属材料有限责任公司 | A kind of metal fiber cloth and its preparation method and application |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1900345A (en) * | 2006-07-21 | 2007-01-24 | 周建华 | Metal fiber wire and its producing process |
| CN101220449A (en) * | 2008-01-25 | 2008-07-16 | 湖南惠同新材料股份有限公司 | Fire resistant iron chromium aluminum filament and production technique |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AUPN191395A0 (en) * | 1995-03-22 | 1995-04-27 | M.I.M. Holdings Limited | Atmospheric mineral leaching process |
| CN100554452C (en) * | 2008-07-17 | 2009-10-28 | 北京矿冶研究总院 | Method for extracting copper from copper-containing sulfide ore by wet process |
| CN102477577A (en) * | 2010-11-22 | 2012-05-30 | 湖南汇博金属材料有限责任公司 | Preparation process for metal fibers |
| CN103572068A (en) * | 2012-08-02 | 2014-02-12 | 厦门紫金矿冶技术有限公司 | Method for recovering copper from copper-containing gold-loaded carbon |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1900345A (en) * | 2006-07-21 | 2007-01-24 | 周建华 | Metal fiber wire and its producing process |
| CN101220449A (en) * | 2008-01-25 | 2008-07-16 | 湖南惠同新材料股份有限公司 | Fire resistant iron chromium aluminum filament and production technique |
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Address after: No. 8, Yuanshan Road, Eastern New Area, Heshan District, Yiyang City, Hunan Province Patentee after: HUNAN HUIBO METAL MATERIAL Co.,Ltd. Patentee after: NV BEKAERT S.A. Address before: 413064 No. 8, Yuanshan Road, Eastern New Area, Heshan District, Yiyang City, Hunan Province Patentee before: HUNAN HUIBO METAL MATERIAL Co.,Ltd. Patentee before: Bei Kaerte |
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Effective date of registration: 20220511 Address after: 413064 No. 8, Yuanshan Road, Eastern New Area, Heshan District, Yiyang City, Hunan Province Patentee after: HUNAN HUIBO METAL MATERIAL Co.,Ltd. Patentee after: Bei Kaerte Address before: 413064 No. 8 Yuanshan Road, East New Area, Yiyang City, Hunan Province Patentee before: HUNAN HUIBO METAL MATERIAL Co.,Ltd. |