CN102531027A - Method for preparing heavy basic copper carbonate - Google Patents
Method for preparing heavy basic copper carbonate Download PDFInfo
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- CN102531027A CN102531027A CN2012100260762A CN201210026076A CN102531027A CN 102531027 A CN102531027 A CN 102531027A CN 2012100260762 A CN2012100260762 A CN 2012100260762A CN 201210026076 A CN201210026076 A CN 201210026076A CN 102531027 A CN102531027 A CN 102531027A
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- ammonia
- air
- cuprammonia
- squeezed
- gas
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Abstract
The invention discloses a method for producing heavy basic copper carbonate by a new secondary oxidation copper removal and air stripping process. Copper, ammonia and ammonium bicarbonate are taken as raw materials, and the method comprises the following steps of: performing leaching synthesis reaction, filtering, performing thermal decomposition, separating, washing, drying, crushing, packaging after inspection, and the like. By the preparation method, the decomposition reaction speed is improved, byproducts and waste materials are avoided, the utilization rate of the raw materials is high, environmental pollution is avoided, a problem of water balance in the production process is solved, and the method accords with a sustainable development policy and belongs to a clean production process.
Description
Technical field
The present invention relates to a kind of preparation method of basic cupric carbonate, be specifically related to the method that a kind of secondary oxidation copper removal and air gas are carried explained hereafter heavy ventilation breather.
Background technology
The heavy ventilation breather belongs to field of fine chemical, is mainly used in organic catalyst, sterilant, and electronic ceramics, crude oil is stored dealkalize agent etc.It is raw material with copper, ammonia, bicarbonate of ammonia that prior art provides a kind of; The method for preparing the heavy ventilation breather through technical process such as strong aqua preparation, leaching building-up reactions, filtration, thermolysis, separation, oven dry, pulverizing, test packages; In changing the copper process, can generate a certain amount of copper powder inevitably, the space of depositing copper powder, periodic cleaning are left in traditionization copper pond below card; It is little to rouse air capacity simultaneously, so that the sinking of copper powder; Filter and use natural filtration, prevent that copper powder from penetrating, cause disproportionation reaction takes place when thermolysis, so oxidation generation cupric oxide, make the product blackout, off quality.This technology existenceization copper speed is slow, and cleaning copper powder labor capacity is big, and natural filtration speed is slow and ammonia is seriously polluted.In thermal decomposition process, adopt and directly feed steam heating, consequently vapor condensation causes that mother liquor expands, and mother liquor is retrieval system all; Water is seriously polluted, the raw material recovery is low; The weighing apparatus that can not be up to the standard must be produced other products separately, makes flow process complicated; By-product brings certain difficulty to sale simultaneously.
Summary of the invention
The present invention provides a kind of secondary oxidation copper removal and air gas to put forward the method for explained hereafter heavy ventilation breather in order to overcome the shortcoming that prior art exists.This preparation method has improved decomposition reaction velocity, and does not have sub product and waste material generation, and raw material availability is high, and non-environmental-pollution has solved water balance problem in the production process, meets the Sustainable development policy, belongs to process for cleanly preparing.
Concrete process method of the present invention is:
(1) leaching building-up reactions: with concentration is that 10～12% ammoniacal liquor is squeezed into the Hua Tongchi that copper wire or copper scale are housed, and presses NH
4HCO
3/ NH
3Mol ratio>=2 add bicarbonate of ammonia, blast air with air compressor machine, and control reaction temperature is 60 ℃～70 ℃, and reaction formula is: Cu+NH
4HCO
3+ NH
3+ 1/20
2=Cu (NH
3)
2CO
3+ H
2O;
(2) filter: after with pump 3/4 cuprammonia of step (1) being squeezed into telescopic strainer filtration, cuprammonia flows into reaction kettle;
(3) thermolysis: in reaction kettle, blast air with air compressor machine, and be warmed up to 80 ℃～100 ℃, carry out that secondary oxidation is gentle to be carried, remove the copper powder in the cuprammonia, pyrolysis: 2Cu (NH
3)
2CO
3+ H
2O → CuCO
3.Cu (OH)
2↓+4NH
3+ CO
2, gas is sent into condensing surface and is reclaimed;
(4) separate, wash: after treating cuprammonia pH value≤9.0 of step (3), squeeze into storage tank, carry out spinning, washing then with pump;
(5) the ventilation breather filter cake that step (4) is obtained through oven dry, pulverize, the qualified back of chemical examination packs.
Further improvement project of the present invention is; Contain water vapor, ammonia and carbonic acid gas with the air admission condensing surface in the gas that step (3) thermolysis is come out; Part ammonia and carbonic acid gas get into phlegma and generate carbonated aqueous ammonia during condensation; Carbonated aqueous ammonia is squeezed into the residual air that the absorption tower absorptive condenser is come after cooling, the carbonated aqueous ammonia after the absorption reclaims system strong aqua, micro-ammonia burning and exhausting in the tail gas from absorption tower; Mother liquor and dense washing lotion after step (4) washing are squeezed into Hua Tongchi, and light washing lotion reclaims the system strong aqua.
The present invention compared with prior art has following obvious advantage:
1, filtration step of the present invention is owing to adopt the jacket casing strainer that two big advantages are arranged, and the one, filtration velocity is very fast, and the 2nd, material is not walked in sleeve and is contacted with air, thereby does not have the effusion of ammonia, has solved air pollution problems inherent.
2, secondary oxidation copper removal and air gas are put forward technology, have removed the copper powder that penetrates from telescopic strainer, at NH
4HCO
3And NH
3Under the condition that exists, generate ammonia formula verditer, stoped the carrying out of disproportionation reaction, thereby solved product blackout problem.
3, warm air gas is carried and is caught up with ammonia, has shortened the pyrolysis required time, at similarity condition 10m
3In the reaction kettle, carrying required time without air gas is 70 hours, carries the time with air gas and only needs 20 hours, and decomposition rate has improved more than three times, thereby has improved plant factor.
4, air gas is proposed heating and has been solved mother liquor expansible problem, makes whole mother liquors and most of washing lotion retrieval system, recycles, thereby is up to the standard weighing apparatus.
Facts have proved that 5, strengthen the air consumption, it is fast to remove free ammonia speed, thereby make the cuprammonia of PH＞9 originally reach the best crystallization condition of the heavy ventilation breather of PH≤9 very soon, product proportion is increased;
6, air gas is lifted to flexible stirring action, can promptly save power consumption without the rigidity whisking appliance, makes the product particle chap again, helps separating and washing.
7, warm air gas is carried the direct heating material, has saved steam consumption, has practiced thrift the energy.
8, the carbonated aqueous ammonia on absorption tower is recycled, and tail gas contains micro-ammonia burning and exhausting (ammonia limits of explosion 16～27%, ammonia is far below this limit, so can not explode in the tail gas), has solved air pollution problems inherent.
Description of drawings
Fig. 1 is a heavy ventilation breather technological process of production synoptic diagram of the present invention.
Embodiment
Below in conjunction with accompanying drawing the present invention is further described:
Embodiment 1:Referring to accompanying drawing, technical process of the present invention is following:
(1) strong aqua preparation: preparing concentration with deionized water and liquefied ammonia (or rare carbonated aqueous ammonia on recovery absorption tower with separate light washing lotion) is 11% ammoniacal liquor,
(2) leaching building-up reactions: the strong aqua of step (1) is squeezed into the Hua Tongchi that copper wire is housed, press NH
4HCO
3/ NH
3Mol ratio=2 add bicarbonate of ammonia, blast air with air compressor machine, and using the steam control reaction temperature then is 60 ℃, causes reaction solution and meets sulfuric acid test (promptly reacting).
Sulfuric acid test is: get the about 5ml of clear liquid, add sulphate reagent and must not produce red precipitate.
Detect principle: Cu (NH
3)
2CO
3+ H
2SO
4→ CuSO
4Blue look solution is explained and is reacted,
Cu (OH)
2CO
3+ H
2SO
4→ CuSO
4+ Cu ↓ red unreacted is good
The building-up reactions formula is: Cu+NH
4HCO
3+ NH
3+ 1/20
2=Cu (NH
3)
2CO
3+ H
2O
(3) filter: after with pump 3/4 cuprammonia in the step (2) being squeezed into telescopic strainer filtration, flow into reaction kettle, change and stay 1/4 cuprammonia to make following batch of disproportionation reaction accelerationization copper speed in the copper pond.
(4) thermolysis: (outlet air temperature is roughly at 40 ℃-50 ℃ in reaction kettle, to blast air with air compressor machine; The pressure of air compressor machine is the 6-8 kilogram); And be warmed up to 80 ℃ (used vapour indirect heating); Carry out that secondary oxidation is gentle to be carried, remove and filter the copper powder that penetrates, carry out pyrolysis this moment: 2Cu (NH
3)
2CO
3+ H
2O → CuCO
3.Cu (OH)
2↓+4NH
3+ CO
2
Contain water vapor, ammonia and carbonic acid gas in the gas that thermolysis is come out with the air admission condensing surface; Part ammonia and carbonic acid gas get into phlegma and generate carbonated aqueous ammonia during condensation; Carbonated aqueous ammonia is squeezed into the residual air that the absorption tower absorptive condenser is come after cooling; Carbonated aqueous ammonia after the absorption is sent the strong aqua preparation vessel back to, and micro-ammonia is sent into the boiler combustion discharging with gas blower in the tail gas from absorption tower.
(5) separate, washing: treat cuprammonia pH value=9.0 o'clock in the step (4), squeeze into storage tank, carry out spinning, washing then, isolate ventilation breather filter cake, mother liquor, dense washing lotion, light washing lotion with pump.Mother liquor and dense washing lotion are squeezed into Hua Tongchi, and light washing lotion is squeezed into strong aqua preparation vessel system.
(6) oven dry
(7) pulverize
(8) the qualified back of chemical examination packing.
Obtain the technical indicator of product
Embodiment 2:The main technique method is with example 1, and wherein, second step was pressed NH
4HCO
3/ NH
3Mol ratio=3 adds bicarbonate of ammonia, and temperature of reaction is 70 ℃, and the thermolysis Heating temperature in the 4th step is 100 ℃, and the 5th step treated to separate thermolysis cuprammonia pH value=8.0 o'clock, wash, dry, pulverize, pack after the assay was approved.
Claims (3)
1. heavy preparation method of basic cupric carbonate is characterized in that: may further comprise the steps,
(1) leaching building-up reactions: with concentration is that 10～12% ammoniacal liquor is squeezed into the Hua Tongchi that copper wire or copper scale are housed, and presses NH
4HCO
3/ NH
3Mol ratio>=2 add bicarbonate of ammonia, blast air with air compressor machine, and control reaction temperature is 60 ℃～70 ℃, and reaction formula is: Cu+NH
4HCO
3+ NH
3+ 1/20
2=Cu (NH
3)
2CO
3+ H
2O;
(2) filter: after with pump 3/4 cuprammonia of step (1) being squeezed into telescopic strainer filtration, cuprammonia flows into reaction kettle;
(3) thermolysis: in reaction kettle, blast air with air compressor machine, and be warmed up to 80 ℃～100 ℃, carry out that secondary oxidation is gentle to be carried, remove the copper powder in the cuprammonia, pyrolysis: 2Cu (NH
3)
2CO
3+ H
2O → CuCO
3.Cu (OH)
2↓+4NH
3+ CO
2, gas is sent into condensing surface and is reclaimed;
(4) separate, wash: after treating cuprammonia pH value≤9.0 of step (3), squeeze into storage tank, carry out spinning, washing then with pump;
(5) the ventilation breather filter cake that step (4) is obtained through oven dry, pulverize, the qualified back of chemical examination packs.
2. a kind of heavy preparation method of basic cupric carbonate according to claim 1; It is characterized in that: contain water vapor, ammonia and carbonic acid gas with the air admission condensing surface in the gas that step (3) thermolysis is come out; Part ammonia and carbonic acid gas generate carbonated aqueous ammonia during condensation; Carbonated aqueous ammonia is squeezed into the residual air that the absorption tower absorptive condenser is come after cooling, the carbonated aqueous ammonia after the absorption reclaims system strong aqua, micro-ammonia burning and exhausting in the tail gas from absorption tower.
3. a kind of heavy preparation method of basic cupric carbonate according to claim 1 and 2 is characterized in that: mother liquor and dense washing lotion after step (4) washing are squeezed into Hua Tongchi, and light washing lotion reclaims the system strong aqua.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012100260762A CN102531027A (en) | 2012-02-07 | 2012-02-07 | Method for preparing heavy basic copper carbonate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012100260762A CN102531027A (en) | 2012-02-07 | 2012-02-07 | Method for preparing heavy basic copper carbonate |
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|---|---|
| CN102531027A true CN102531027A (en) | 2012-07-04 |
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ID=46339248
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|---|---|---|---|
| CN2012100260762A Pending CN102531027A (en) | 2012-02-07 | 2012-02-07 | Method for preparing heavy basic copper carbonate |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103011248A (en) * | 2012-12-21 | 2013-04-03 | 泰兴冶炼厂有限公司 | Method for preparing heavy high-purity basic cupric carbonate |
| CN103011246A (en) * | 2012-12-21 | 2013-04-03 | 泰兴冶炼厂有限公司 | Method for preparing heavy high-purity basic cupric carbonate |
| CN103011247A (en) * | 2012-12-21 | 2013-04-03 | 泰兴冶炼厂有限公司 | Method for preparing heavy highly-pure basic cupric carbonate |
| CN115124066A (en) * | 2022-07-22 | 2022-09-30 | 李晓清 | Continuous production process of basic copper carbonate based on ammonia circulation system |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1082004A (en) * | 1992-08-12 | 1994-02-16 | 黄石市能源综合科学技术研究所 | Produce a kind of efficient process of ventilation breather or cupric oxide |
| CN1172074A (en) * | 1997-08-15 | 1998-02-04 | 张礼英 | Preparation method of cupric oxide or cupric sulfate using copper sheathed steel by ammonia immersion |
| CN101984097A (en) * | 2010-11-24 | 2011-03-09 | 苏州市环境工程有限责任公司 | Method for comprehensive recovery of heavy metal from spent solder stripper |
-
2012
- 2012-02-07 CN CN2012100260762A patent/CN102531027A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1082004A (en) * | 1992-08-12 | 1994-02-16 | 黄石市能源综合科学技术研究所 | Produce a kind of efficient process of ventilation breather or cupric oxide |
| CN1172074A (en) * | 1997-08-15 | 1998-02-04 | 张礼英 | Preparation method of cupric oxide or cupric sulfate using copper sheathed steel by ammonia immersion |
| CN101984097A (en) * | 2010-11-24 | 2011-03-09 | 苏州市环境工程有限责任公司 | Method for comprehensive recovery of heavy metal from spent solder stripper |
Non-Patent Citations (1)
| Title |
|---|
| 樊雨杰等: "二次氧化除铜和空气气提生产重质碱式碳酸铜新工艺", 《科技成果》, 23 January 2003 (2003-01-23) * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103011248A (en) * | 2012-12-21 | 2013-04-03 | 泰兴冶炼厂有限公司 | Method for preparing heavy high-purity basic cupric carbonate |
| CN103011246A (en) * | 2012-12-21 | 2013-04-03 | 泰兴冶炼厂有限公司 | Method for preparing heavy high-purity basic cupric carbonate |
| CN103011247A (en) * | 2012-12-21 | 2013-04-03 | 泰兴冶炼厂有限公司 | Method for preparing heavy highly-pure basic cupric carbonate |
| CN115124066A (en) * | 2022-07-22 | 2022-09-30 | 李晓清 | Continuous production process of basic copper carbonate based on ammonia circulation system |
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Application publication date: 20120704 |