CN103253716B - New technology of recycling ammonium bicarbonate during production of cobaltosic oxide - Google Patents

New technology of recycling ammonium bicarbonate during production of cobaltosic oxide Download PDF

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CN103253716B
CN103253716B CN201310228528.XA CN201310228528A CN103253716B CN 103253716 B CN103253716 B CN 103253716B CN 201310228528 A CN201310228528 A CN 201310228528A CN 103253716 B CN103253716 B CN 103253716B
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gas
carbonization
ammonia
cobalt carbonate
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CN103253716A (en
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谢福标
蒋光勤
吴阳红
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Ganzhou Teng far cobalt new materials Limited by Share Ltd
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GANZHOU TENGYUAN COBALT INDUSTRIAL Co Ltd
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Abstract

A new technology of recycling ammonium bicarbonate during production of cobaltosic oxide is characterized in that weak aqua ammonia generated by treating waste water containing ammonia nitrogen absorbs carbon dioxide generated when cobaltosic oxide is roasted by cobalt carbonate to synthesize an ammonium bicarbonate solution, and the ammonium bicarbonate solution is recycled in a synthesis process of cobalt carbonate. The technology can effectively realize resource recycling of ammonium bicarbonate, lowers the production cost, is energy-saving and environment-friendly, can effectively reduce the labor intensity of related workers, improves the labor efficiency and has better social and economic benefits.

Description

In a kind of cobaltosic oxide production process, recycle the technique of carbonic hydroammonium
Technical field
The invention belongs to the comprehensive utilization of resources technology in industrial chemicals preparation field, be specially a kind of for utilizing cobalt carbonate to recycle the new technology of carbonic hydroammonium prepare the cobaltosic oxide production process that cobaltosic oxide produces as raw material in.
Background technology
Cobaltosic oxide powder purposes is very extensive, and its purposes comprises piezo-resistance, gas sensor sensing element, magnetic material, ultracapacitor, catalyst, optical material, anode material for lithium-ion batteries etc.
The preparation method of cobaltosic oxide is a lot, wherein in wet-precipitated-solid-phase pyrolysis, with ammonium bicarbonate precipitation cobalt chloride solution, prepare the production technology that cobaltosic oxide is prepared in cobalt carbonate presoma and then calcining, because this method has reaction condition gentleness, technique is simple, product composition is even and purity high, it is one of main production method current and one period from now on.
Existing cobalt carbonate-cobaltosic oxide technology is as follows:
Building-up process reaction equation
2CoCl 2+5NH 4HCO 3 = 2CoCO 3↓+4NH 4Cl(L)+3CO 2+3H 2O+NH 3
--------------------①
Waste water concentrating, evaporation, crystallization process reaction equation
NH 4Cl(L) = NH 4Cl(S)↓ -------------------②
Calcination process reaction equation
3CoCO 3+ 1/2 O 2 = Co 3O 4 + 3CO 2↑ -------------------③
From reaction equation, 1. can find out, in building-up process, will constantly add new carbonic hydroammonium, and produce a large amount of ammonium chloride waste-waters; Waste water need to be after solid ammonium chloride product be produced in reaction equation concentrated, evaporation, crystallization 2. qualified discharge; Reaction equation 3. cobalt carbonate calcination process produces a large amount of carbon dioxide greenhouse gas and drains in atmosphere.
The shortcoming that above-mentioned process route exists has:
1, in building-up process, need constantly to add new carbonic hydroammonium;
2, cobalt carbonate calcination process produces a large amount of carbon dioxide greenhouse gas and drains in atmosphere;
3, ammonia nitrogen resource does not obtain most economical, reasonably utilization;
4, need dissolved solid carbonic hydroammonium operation.
Summary of the invention
Technical problem solved by the invention is to provide the new technology that recycles carbonic hydroammonium in a kind of cobaltosic oxide production process, to solve the shortcoming in above-mentioned background technology.
Technical problem solved by the invention realizes by the following technical solutions:
In a kind of cobaltosic oxide production process, recycle the new technology of carbonic hydroammonium, the weak aqua ammonia that utilizes processing nitrogen-containing wastewater to produce removes to absorb the carbon dioxide producing in cobalt carbonate calcining cobaltosic oxide process and carrys out carbonate synthesis hydrogen ammonium salt solution, and this ammonium bicarbonate soln recirculation is used in cobalt carbonate building-up process.Building-up process reaction equation in its technology is as follows:
2CoCl 2+5NH 4HCO 3 = 2CoCO 3↓+4NH 4Cl(L)+3CO 2↑+3H 2O+NH 3↑ --------①
Calcination process reaction equation
3CoCO 3+ 1/2 O 2 = Co 3O 4 + 3CO 2↑ -------------------②
Wastewater treatment reaction equation
CaO+H 2O=Ca(OH) 2 ----------------③
NH 4Cl(L) + Ca(OH) 2 = CaCl 2 + NH 3↑+ H 2O -------------------④
NH 3+ H 2o=NH 3h 2o(weak aqua ammonia)-------------------5.
NH 3h 2o(weak aqua ammonia)+CO 2=NH 4hCO 3(L)-------------------6.
Concrete technology process description is as follows:
1, cobalt carbonate is synthetic
2CoCl 2+5NH 4HCO 3 = 2CoCO 3↓+4NH 4Cl(L)+3CO 2↑+3H 2O+NH 3↑ --------①
In cobalt carbonate building-up process, carbonic hydroammonium is from the ammonium bicarbonate soln producing in wastewater treatment process, and concentration can regulate and control as required, thereby does not have solid ammonium bicarbonate to dissolve this process.
2, cobalt carbonate calcining cobaltosic oxide process
3CoCO 3+ 1/2 O 2 = Co 3O 4 + 3CO 2↑ -------------------②
The reaction that calcination process occurs is constant, yet airtight, the retracting device that in calciner, increase carbon dioxide reach and reclaim carbon dioxide for synthetic fluid carbonic hydroammonium.
3, wastewater treatment process
A, first white lime is added to water and carry out nitratedly, white lime is converted into sulfide lime, course of reaction is as follows:
CaO+H 2O=Ca(OH) 2 ----------------③
B, above-mentioned sulfide lime add reaction tower fully to react with the high strength ammonium-chloride wastewater producing from cobalt carbonate building-up process according to the material ratio of calculating, and utilize vaporizing extract process that the ammonia of reaction generation is converted into gaseous state by liquid state and enter water spray-absorption device generation weak aqua ammonia for next procedure.
NH 4Cl(L) + Ca(OH) 2 = CaCl 2 + NH 3↑+ H 2O -------------------④
NH 3+ H 2o=NH 3h 2o(weak aqua ammonia)-------------------5.
4, carbonic hydroammonium is synthetic
A, carbon dioxide purify, supercharging
By the carbon dioxide gas mixture reclaiming from calcination process, deoxygenation purifies, and oxygen removal process adopts the pressure swing adsorption method deoxygenation in physical deoxidize method, and in this process, the total technological process of gas is: CO 2gaseous mixture through mist supercharger, be pressurized to and under 0.6MPa, enter pressure-variable adsorption deaerating plant, the CO resolving under normal pressure 2gas is again by CO 2compressor pressurizes is entered carbonic hydroammonium process units to 0.3MPa.
Synthesizing of B, carbonic hydroammonium
Gas flow process: from CO 2the unstripped gas of compressor is introduced into gas-liquid separator, isolate and from carbonization king-tower bottom, enter carbonization king-tower after condensate liquid and ammoniacal liquor carries out carburizing reagent, reacted gas from carbonization king-tower top out, then enters carbonization secondary tower from carbonization secondary tower bottom and reacts with the ammoniacal liquor in secondary tower.Then gas goes out from the top of carbonization secondary tower, then the bottom of entering ammonia recovery tower enters ammonia recovery tower, and gas directly contacts with top-down soft water in tower in ammonia recovery tower, in gas recovery with ammonia.Last gas from ammonia recovery tower top out, enters bubble absorbing tower and absorbs again tail gas ammonia in gas, goes out the gas of bubble tower discharged to atmosphere.
Ammoniacal liquor flow process: from the weak aqua ammonia of wastewater treatment operation, enter ammoniacal liquor storage tank.By aqua ammonia pump, from the top of secondary carbonators, send into secondary carbonators again, ammoniacal liquor contacts with gas from bottom to top in secondary carbonators, absorbs the CO in gas 2, then absorb CO 2ammoniacal liquor by carbonization pump, from secondary carbonators, extract the top that is sent to main carbonators out again and enter carbonization king-tower, ammoniacal liquor contacts with gas from bottom to top in carbonization king-tower, with the CO in gas 2carry out carburizing reagent and generate carbonic hydroammonium.Reacted ammonium bicarbonate soln is out sent battery limit (BL) at the bottom of the tower of carbonization king-tower, returns to the reuse of cobalt carbonate synthesis procedure, and chemical formula can be expressed as:
NH 3h 2o(weak aqua ammonia)+CO 2=NH 4hCO 3(L)-------------------6..
Advantage of the present invention and beneficial effect are:
1, technical process consumes cheap white lime, by mineralized nitrogen in the ammonium chloride solution of high concentration, be ammoniacal liquor, absorb the carbon dioxide that calcination process produces, carbonate synthesis hydrogen ammonium salt solution, be back to use in the synthesis procedure of cobalt carbonate, the resource reutilization of having accomplished carbonic hydroammonium, has reduced production cost;
2, the discharge capacity that greatly reduces carbon dioxide greenhouse gas, turns waste into wealth carbon dioxide to be utilized, and for national energy-saving reduces discharging, contributes;
3, cancel the dissolution process of solid ammonium bicarbonate, reduced labour intensity, improved efficiency.
Accompanying drawing explanation
Fig. 1 is schematic diagram of the present invention.
The specific embodiment
Give an actual example and describe the present invention below.
1, cobalt carbonate is synthetic
2CoCl 2+5NH 4HCO 3 = 2CoCO 3↓+4NH 4Cl(L)+3CO 2↑+3H 2O+NH 3↑ --------①
In cobalt carbonate building-up process, reaction equation is constant with old technique, and the technical indicator that cobalt chloride solution and building-up process are controlled is also the same with old technique, but carbonic hydroammonium source is just different.Carbonic hydroammonium in old technique, from outsourcing solid ammonium bicarbonate, need to be dissolved in water and reach the concentration solution that technic index requires; The carbonic hydroammonium of new technology is from the ammonium bicarbonate soln producing in wastewater treatment process, and concentration can regulate and control as required, does not have solid ammonium bicarbonate to dissolve this process.
2, cobalt carbonate calcining cobaltosic oxide process
3CoCO 3+ 1/2 O 2 = Co 3O 4 + 3CO 2↑ -------------------②
The reaction that calcination process occurs is constant, and the technical indicator of process control is also the same with old technique; Airtight, retracting device that new technology increases carbon dioxide in calciner reach recovery carbon dioxide for synthetic fluid carbonic hydroammonium.
3, wastewater treatment process
The white lime of A, outside buying, first adds water and carries out nitratedly, and white lime is converted into sulfide lime, and course of reaction is as follows:
CaO+H 2O=Ca(OH) 2 ----------------③
B, above-mentioned sulfide lime add reaction tower fully to react with the high strength ammonium-chloride wastewater producing from cobalt carbonate building-up process according to the material ratio of calculating, and utilize vaporizing extract process that the ammonia of reaction generation is converted into gaseous state by liquid state and enter water spray-absorption device generation weak aqua ammonia for next procedure.
NH 4Cl(L) + Ca(OH) 2 = CaCl 2 + NH 3↑+ H 2O -------------------④
NH 3+ H 2o=NH 3h 2o(weak aqua ammonia)-------------------5.
4, carbonic hydroammonium is synthetic
A, carbon dioxide purify, supercharging
The carbon dioxide gas mixture reclaiming from calcination process, because oxygen content is very high, that the ammonia in material liquid ammoniacal liquor belongs to is inflammable, easy sudden and violent, fuel gas, must first carbon dioxide gas mixture deoxygenation be purified.
Deoxygenation adopts physical deoxidize---pressure swing adsorption method deoxygenation.Pressure-variable adsorption deoxygenation is to adsorb under 0.6MPa pressure, resolves O under normal pressure 2content drop to safety index scope below 0.5%, CO 2the rate of recovery can reach more than 85%.
Due to CO 2gaseous mixture be normal temperature and pressure, therefore supercharger need be set by CO 2gaseous mixture be pressurized to the required pressure of pressure swing adsorption method deoxygenation.
The CO parsing 2gas is normal pressure, in order to overcome the resistance in ammonium hydrogencarbonate production process, therefore need set up carbon dioxide mix gas supercharger, carbon dioxide mix gas is pressurized to 0.30MPa by normal pressure, then enters production process.
As shown in Figure 1, it specifically can be expressed as the total technological process sketch of gas: CO 2gaseous mixture through mist supercharger, be pressurized to and under 0.6MPa, enter pressure-variable adsorption deaerating plant, the CO resolving under normal pressure 2gas is again by CO 2compressor pressurizes is entered carbonic hydroammonium process units to 0.3MPa.
Synthesizing of B, carbonic hydroammonium
Gas flow process: from CO 2the unstripped gas of compressor is introduced into gas-liquid separator, isolate and from carbonization king-tower bottom, enter carbonization king-tower after condensate liquid and ammoniacal liquor carries out carburizing reagent, reacted gas from carbonization king-tower top out, then enters carbonization secondary tower from carbonization secondary tower bottom and reacts with the ammoniacal liquor in secondary tower.Then gas goes out from the top of carbonization secondary tower, then the bottom of entering ammonia recovery tower enters ammonia recovery tower, and gas directly contacts with top-down soft water in tower in ammonia recovery tower, in gas recovery with ammonia.Last gas from ammonia recovery tower top out, enters bubble absorbing tower and absorbs again tail gas ammonia in gas, goes out the gas of bubble tower discharged to atmosphere.
Ammoniacal liquor flow process: from the weak aqua ammonia of wastewater treatment operation, enter ammoniacal liquor storage tank.By aqua ammonia pump, from the top of secondary carbonators, send into secondary carbonators again, ammoniacal liquor contacts with gas from bottom to top in secondary carbonators, absorbs the CO in gas 2, then absorb CO 2ammoniacal liquor by carbonization pump, from secondary carbonators, extract the top that is sent to main carbonators out again and enter carbonization king-tower, ammoniacal liquor contacts with gas from bottom to top in carbonization king-tower, with the CO in gas 2carry out carburizing reagent and generate carbonic hydroammonium.Reacted ammonium bicarbonate soln is out sent battery limit (BL) at the bottom of the tower of carbonization king-tower, returns to the reuse of cobalt carbonate synthesis procedure, and its chemical formula can be expressed as:
NH 3h 2o(weak aqua ammonia)+CO 2=NH 4hCO 3(L)-------------------6..
More than show and described basic principle of the present invention and principal character and advantage of the present invention.The technical staff of the industry should understand; the present invention is not restricted to the described embodiments; that in above-described embodiment and description, describes just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.The claimed scope of the present invention is defined by appending claims and equivalent thereof.

Claims (2)

1. in a cobaltosic oxide production process, recycle the technique of carbonic hydroammonium, it is characterized in that the weak aqua ammonia that utilizes processing nitrogen-containing wastewater to produce goes absorption calcining cobalt carbonate to prepare the carbon dioxide producing in cobaltosic oxide process and carrys out carbonate synthesis hydrogen ammonium salt solution, and this ammonium bicarbonate soln recirculation is used in cobalt carbonate building-up process, its operating procedure step comprises:
1), cobalt carbonate is synthetic;
2), calcining cobalt carbonate is prepared cobaltosic oxide;
3), wastewater treatment process;
4), carbonic hydroammonium is synthetic;
The technological process of its wastewater treatment process is as follows:
1), first quick lime is added to water and digests, quick lime is converted into calcium hydroxide;
2), above-mentioned calcium hydroxide adds reaction tower fully to react with the high strength ammonium-chloride wastewater producing from cobalt carbonate building-up process according to material ratio, utilize ammonia that vaporizing extract process generates reaction to be converted into gaseous state by liquid state and enter water spray-absorption device and generate weak aqua ammonia for next procedure;
The technological process of the building-up process of its carbonic hydroammonium is as follows:
1), carbon dioxide purification, supercharging
By the carbon dioxide gas mixture reclaiming from calcination process, deoxygenation purifies, and oxygen removal process adopts the pressure swing adsorption method deoxygenation in physical deoxidize method, and in this process, the total technological process of gas is:
CO 2gaseous mixture through mist supercharger, be pressurized to and under 0.6MPa, enter pressure-variable adsorption deaerating plant, the CO resolving under normal pressure 2gas is again by CO 2compressor pressurizes is entered carbonic hydroammonium process units to 0.3MPa;
2), carbonic hydroammonium is synthetic
Gas flow process: from CO 2the unstripped gas of compressor is introduced into gas-liquid separator, isolate and from carbonization king-tower bottom, enter carbonization king-tower after condensate liquid and ammoniacal liquor carries out carburizing reagent, reacted gas from carbonization king-tower top out, then enters carbonization secondary tower from carbonization secondary tower bottom and reacts with the ammoniacal liquor in secondary tower; Then gas goes out from the top of carbonization secondary tower, then the bottom of entering ammonia recovery tower enters ammonia recovery tower, and gas directly contacts with top-down soft water in tower in ammonia recovery tower, in gas recovery with ammonia; Last gas from ammonia recovery tower top out, enters bubble absorbing tower and absorbs again tail gas ammonia in gas, goes out the gas of bubble tower discharged to atmosphere;
Ammoniacal liquor flow process: from the weak aqua ammonia of wastewater treatment operation, enter ammoniacal liquor storage tank, then send into carbonization secondary tower by aqua ammonia pump from the top of carbonization secondary tower, ammoniacal liquor contacts with gas from bottom to top in carbonization secondary tower, absorbs the CO in gas 2, then absorb CO 2ammoniacal liquor by carbonization pump, from carbonization secondary tower, extract the top be sent to carbonization king-tower out again and enter carbonization king-tower, ammoniacal liquor contacts with gas from bottom to top in carbonization king-tower, with the CO in gas 2carry out carburizing reagent and generate carbonic hydroammonium, reacted ammonium bicarbonate soln is out sent battery limit (BL) at the bottom of the tower of carbonization king-tower, returns to the reuse of cobalt carbonate synthesis procedure.
2. in a kind of cobaltosic oxide production process according to claim 1, recycle the technique of carbonic hydroammonium, it is characterized in that, described calcining cobalt carbonate is prepared to increase in the calciner that cobaltosic oxide process uses to be had airtight, the retracting device of carbon dioxide to reach to reclaim carbon dioxide for carbonate synthesis hydrogen ammonium salt solution.
CN201310228528.XA 2013-06-09 2013-06-09 New technology of recycling ammonium bicarbonate during production of cobaltosic oxide Active CN103253716B (en)

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Address after: 341100 Jiangxi city of Ganzhou province Ganxian County Hongjin Industrial Zone

Patentee after: Ganzhou Teng far cobalt new materials Limited by Share Ltd

Address before: 341100 Jiangxi city of Ganzhou province Ganxian County Hongjin Industrial Zone

Patentee before: Ganzhou Tengyuan Cobalt Industrial Co., Ltd.