CN102515253B - Production method for producing zinc oxide by ammonia process and comprehensively utilizing waste water - Google Patents
Production method for producing zinc oxide by ammonia process and comprehensively utilizing waste water Download PDFInfo
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- CN102515253B CN102515253B CN 201210001840 CN201210001840A CN102515253B CN 102515253 B CN102515253 B CN 102515253B CN 201210001840 CN201210001840 CN 201210001840 CN 201210001840 A CN201210001840 A CN 201210001840A CN 102515253 B CN102515253 B CN 102515253B
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Abstract
The invention aims to provide a process technique for producing zinc oxide by an ammonia process and comprehensively utilizing waste water and complete equipment for realizing the technique. In particular, a zinc ammonia solution prepared by dissolving zinc ore powder in water is used as a raw material, a novel energy-saving technique is used to prepare high-purity zinc oxide, and the ammonia in the zinc ammonia solution is recovered and prepared into ammonia water; and thus, production waste water is comprehensively recovered and reduced, the ammonia discharge concentration in tail gas is lowered, the pollution of production to the ecological environment is reduced, and zinc oxide is produced in an environment-friendly manner.
Description
Technical field
The present invention relates to a kind of isolation technique and suite of equipment of chemical industry, the Technology of zinc ammoniacal liquor recycling and realize the suite of equipment of this technology in a kind of ammonia process zinc oxide production specifically.
Background technology
Zinc oxide is a kind of important chemical material, all has a wide range of applications in industries such as rubber, medicine, makeup, weaving, electronics, material.The production of zinc oxide generally can be divided into direct method and indirect method, and direct method adopts roasting-leaching two step process mostly, and this method can produce a large amount of obnoxious flavoures, and environmental pollution is more serious, exists the waste of resource simultaneously; Using at present more is indirect method, comprises ammonia-volatile salt method and ammonia lixiviation process, and ammonia process technology is short because of its flow process, and speed of response is fast, and the quality height pollutes less and is subjected to the favor of factory.
Yet can produce a large amount of waste liquids in the ammonia process zinc oxide production process, directly discharging not only pollutes the environment, and the waste resource; Need a large amount of pure water to wash in the production process simultaneously, the wastewater flow rate that produces is big, difficult treatment, environmental pollution is bigger, and the zinc oxide device overwhelming majority that present China is in production status is on a small scale, does not consider recycling and the measure of energy-saving and emission-reduction consumption reduction of resource, causes the waste of resource and ecological environmental pollution more serious, cause cost high, product does not have price advantage.Proposition along with the social slogan of China's 12 planning constructions " resource-conserving, environmentally friendly ", ammonia process is produced these problems that exist in the zinc oxide process and is caused people's attention gradually, solves utilization of resources and reduce the pollution of discharging, alleviating environment to seem particularly important.
At current this production status, the applicant has invented a kind of environmental protection zinc oxide production technique.This novel process can not only solve the problem of the utilization of resources by efficient recovery zinc oxide, and can realize the comprehensive recycling of waste water, reduces the discharging of the three wastes, reduces the concentration of exhaust emissions, alleviates environmental pollution, has very big economic benefit and social benefit.
Summary of the invention
The object of the present invention is to provide the Technology of a kind of ammonia process zinc oxide production technique and the comprehensive recycling of waste water and realize the suite of equipment of this technology, when can efficient recovery zinc oxide solving the utilization of resources, realize the comprehensive recycling of waste water, reduce the discharging of the three wastes, alleviate environmental pollution, to overcome the defective of prior art.
For achieving the above object, the present invention takes following technical scheme:
A kind of ammonia process zinc oxide is produced the production method with the comprehensive recycling of waste water, it is characterized in that it is made up of ammonia still T101, ammonia desorption tower T102, ammonia recovery tower T103 and filter U1, is undertaken by following step:
(1) from the zinc ammoniacal liquor S1 of dissolving workshop section in ammonia still T101 after distillation is handled dense ammonia distillated by cat head, a part of first strong aqua S3 advances tank used for storing ammonia behind condensation, separatory, thick ammonia S4 enters ammonia recovery tower T103, dense zinc liquid S2 at the bottom of the tower enters among the filter U1,70 ~ 90 ℃ of temperature enter continuation processing recovery ammonia among the ammonia desorption tower T102 through the filter zinc liquid S5 after the filter U1 filtered and recycled zinc oxide component; Wherein ammonia still T101 top is tray column, and the bottom is the herringbone buffle-type tower, and charging is 70 ~ 125 ℃ of the top service temperatures of tower, working pressure 0 ~ 0.2MPa(A); The tray column form that ammonia still T101 adopts can be bubbling class column plate, also can be the ejection-type column plate, and the herringbone baffle plate is single word veneer, double word baffle plate or many herringbones baffle plate; Filter is that flame filter press, whizzer, commentaries on classics are with vacuum filter or strip machine;
(2) contain part ammonia among the filter zinc liquid S5, under the effect of alkali lye S6, handle through ammonia desorption tower T102, the first tail gas S9 emptying after condensation, cooling of cat head component, ammoniacal liquor S8 advances tank used for storing ammonia, further utilize, waste water in the tower has reclaimed active principle after the desorption tower effect, the S7 that purifies waste water at the bottom of the tower has reached emission standard this moment, effluxes; Wherein ammonia desorption tower T102 feed entrance point is the middle and upper part of tower, and the alkali lye import is on top or the middle part, 95 ~ 120 ℃ of service temperatures, working pressure 0 ~ 0.2MPa(A); Ammonia desorption tower T102 can be the Mixed Design tower of tray column, packing tower or column plate and filler; Wherein filter contain ammonia among the zinc liquid S5 concentration less than 2g/L, alkali lye S6 is sodium hydroxide solution;
(3) from the thick ammonia S4 of ammonia still T101, under the effect of process water S10 after ammonia recovery tower T103 absorbs cat head tail gas concentration reduce greatly, the second tail gas S11 emptying, the second strong aqua S12 at the bottom of the tower advances tank used for storing ammonia and does further to utilize, the charging of process water S10 cat head, air inlet at the bottom of the thick ammonia S4 tower; Ammonia recovery tower T103 tower has stage casing circulation heat-obtaining device, 25 ~ 80 ℃ of service temperatures, working pressure 0 ~ 0.2MPa(A); Ammonia recovery tower T103 is the Mixed Design tower of tray column, packing tower or column plate and filler, and stage casing circulation heat-obtaining device has one at least.
Invent described production method, wherein filter contain ammonia among the zinc liquid S5 concentration less than 2g/L, the alkali lye of S6 is sodium hydroxide solution.Adopt technical matters of the present invention can obtain concentration greater than the ammoniacal liquor more than 13%, the recyclable recycling of this ammoniacal liquor, emission intensity concentration is less than 50ppm in the tail gas simultaneously, and process flow diagram is as shown in Figure 1.
The more detailed process treatment process of the present invention following (referring to) Fig. 1:
(1) from the zinc ammoniacal liquor S1 of dissolving workshop section in ammonia still T101 after distillation is handled dense ammonia distillated by cat head, a part of first strong aqua S3 advances tank used for storing ammonia behind condensation, separatory, thick ammonia S4 enters ammonia recovery tower T103, dense zinc liquid S2 at the bottom of the tower enters (70 ~ 90 ℃ of temperature) among the filter U1, enters to continue among the ammonia desorption tower T102 to handle through the filter zinc liquid S5 after the filter U1 filtered and recycled zinc component and reclaims ammonia;
(2) contain part ammonia among the filter zinc liquid S5, under the effect of alkali lye S6, handle through ammonia desorption tower T102, the first tail gas S9 emptying after condensation, cooling of cat head component, ammoniacal liquor S8 advances tank used for storing ammonia, further utilize, waste water in the tower has reclaimed active principle after the desorption tower effect, the S7 that purifies waste water at the bottom of the tower has reached emission standard this moment, effluxes;
(3) from the thick ammonia S4 of T101 ammonia still under the effect of process water S10 after ammonia recovery tower T103 absorbs cat head tail gas concentration reduce greatly, the second tail gas S11 emptying, the second strong aqua S12 at the bottom of the tower advances tank used for storing ammonia and does further to utilize, the charging of process water S10 cat head, air inlet at the bottom of the thick ammonia S4 tower;
The technology features of ammonia process zinc oxide production technique disclosed by the invention and the comprehensive recycling of waste water:
(1) the invention solves that zinc ammoniacal liquor waste water component complexity is difficult to reclaim and the easy difficult problem of polymerization coking occluding device, invented the Technology that a kind of zinc ammoniacal liquor distillation is reclaimed, realized the waste water reclamation recycling that ammonia process zinc oxide is produced, the waste water that reclaims can continue the absorption agent as T103, makes to reclaim behind the ammoniacal liquor and uses.
(2) obtained concentration and be higher than ammoniacal liquor more than 13%, recycling effectively reduces exhaust emissions concentration simultaneously, be not more than 50ppm, reduces environmental pollution.
Description of drawings:
Fig. 1 is the process flow diagram of the comprehensive recycling of zinc ammoniacal liquor waste water; T101 wherein: ammonia still, T102: ammonia desorption tower, T103: ammonia recovery tower, U1: filter, S1: zinc ammoniacal liquor, S2: dense zinc liquid, S3: first strong aqua, S4: thick ammonia, S5: filter zinc liquid, S6: alkali lye, S7: purify waste water S8: ammoniacal liquor, S9: first tail gas, S10: process water, S11: second tail gas, S12: second strong aqua.
Embodiment
Below in conjunction with embodiment the present invention is described, the scheme of embodiment described here, do not limit the present invention, one of skill in the art can make improvements and change according to spirit of the present invention, described these improvement and variation all should be considered as within the scope of the invention, and scope of the present invention and essence are limited by claim.
Embodiment 1
From the zinc ammoniacal liquor S1 of dissolving workshop section in ammonia still T101 after distillation is handled dense ammonia distillated by cat head, a part of first strong aqua S3 advances tank used for storing ammonia behind condensation, separatory, thick ammonia S4 enters ammonia recovery tower T103, dense zinc liquid S2 at the bottom of the tower enters among the filter U1, enters to continue among the ammonia desorption tower T102 to handle through the filter zinc liquid S5 after the filter U1 filtered and recycled zinc component and reclaims ammonia; Contain part ammonia among the filter zinc liquid S5, under the effect of alkali lye (ammonium bicarbonate soln) S6, handle through ammonia desorption tower T102, the first tail gas S9 emptying after condensation, cooling of cat head component, ammoniacal liquor S8 advances tank used for storing ammonia, further utilize, waste water in the tower has reclaimed active principle after the desorption tower effect, the S7 that purifies waste water at the bottom of the tower has reached emission standard this moment, effluxes; From the thick ammonia S4 of T101 ammonia still under the effect of process water S10 after ammonia recovery tower T103 absorbs cat head tail gas concentration reduce (below 50ppm) greatly, the second tail gas S11 emptying, the second strong aqua S12 at the bottom of the tower advances tank used for storing ammonia and does further to utilize, the charging of process water S10 cat head, air inlet at the bottom of the thick ammonia S4 tower.
Zinc ammoniacal liquor S1: concentration 15%, 70 ℃ of feeding temperatures, pressure (gauge pressure) 0.5MPa
Ammonia still T101: sieve-tray tower+single word baffle plate, 30 layers of column plate, 5 layers of herringbone baffle plate, working pressure 0.1 MPa, 40 ~ 110 ℃ of service temperatures
Ammonia desorption tower T102: sieve-tray tower, 40 layers of column plate, working pressure 0.1MPa, 70 ~ 120 ℃ of service temperatures
Ammonia recovery tower T103: packing tower, 6 meters of packed heights, two stage casing circulations, working pressure 0.1MPa, 20 ~ 70 ℃ of service temperatures
Filter: sheet frame pressing machine
The ammonia concentration that reclaims: T101 〉=22%, T102 〉=16%, T103 〉=13%
Exhaust emissions concentration: T102≤50ppm, T103≤48ppm
Device efflux wastewater ammonia nitrogen (free ammonia) is less than 100ppm.
Embodiment 2
According to the technological process among the embodiment 1:
Zinc ammoniacal liquor S1: concentration 14%, 75 ℃ of feeding temperatures, pressure (gauge pressure) 0.5MPa
Ammonia still T101: valve tray+double word baffle plate, 30 layers of column plate, 5 layers of herringbone baffle plate, working pressure 0.1 MPa, 40 ~ 110 ℃ of service temperatures
Ammonia desorption tower T102: valve tray, 40 layers of column plate, working pressure 0.1MPa, 70 ~ 120 ℃ of service temperatures
Ammonia recovery tower T103: valve tray, 30 layers of column plate, two stage casing circulations, working pressure 0.1MPa, 20 ~ 70 ℃ of service temperatures
Filter: whizzer
The ammonia concentration that reclaims: T101 〉=22%, T102 〉=16%, T103 〉=13%
Exhaust emissions concentration: T102≤50ppm, T103≤48ppm
Device efflux wastewater ammonia nitrogen (free ammonia) is less than 100ppm.
Embodiment 3:
According to the technological process among the embodiment 1:
Zinc ammoniacal liquor S1: concentration 18%, 40 ℃ of feeding temperatures, pressure (gauge pressure) 0.4MPa
Ammonia still T101: valve tray+many herringbones baffle plate, 30 layers of column plate, 5 layers of herringbone baffle plate, working pressure 0.1 MPa, 40 ~ 110 ℃ of service temperatures
Ammonia desorption tower T102: packing tower, 15 meters of packed heights, working pressure 0.1MPa, 70 ~ 120 ℃ of service temperatures
Ammonia recovery tower T103: valve tray+filler, 20 layers of column plate, 6 meters high fillers, two stage casing circulations, working pressure 0.1MPa, 20 ~ 70 ℃ of service temperatures
Filter: whizzer
The ammonia concentration that reclaims: T101 〉=22%, T102 〉=16%, T103 〉=13%
Exhaust emissions concentration: T102≤50ppm, T103≤48ppm
Device efflux wastewater ammonia nitrogen (free ammonia) is less than 100ppm.
Embodiment 4:
According to the technological process among the embodiment 1:
Zinc ammoniacal liquor S1: concentration 10%, 75 ℃ of feeding temperatures, pressure (gauge pressure) 0.5MPa
Ammonia still T101: vertical sieve tray column plate+double word baffle plate, 30 layers of column plate, 5 layers of herringbone baffle plate, working pressure 0.1 MPa, 40 ~ 110 ℃ of service temperatures
Ammonia desorption tower T102: vertical sieve tray column plate, 40 layers of column plate, working pressure 0.1MPa, 70 ~ 120 ℃ of service temperatures
Ammonia recovery tower T103: vertical sieve tray column plate, 30 layers of column plate, three stage casing circulations, working pressure 0.1MPa, 20 ~ 70 ℃ of service temperatures
Filter: change same vacuum filter
The ammonia concentration that reclaims: T101 〉=22%, T102 〉=16%, T103 〉=13%
Exhaust emissions concentration: T102≤50ppm, T103≤48ppm
Device efflux wastewater ammonia nitrogen (free ammonia) is less than 100ppm.
Claims (1)
1. an ammonia process zinc oxide is produced the production method with the comprehensive recycling of waste water, it is characterized in that it is made up of ammonia still (T101), ammonia desorption tower (T102), ammonia recovery tower (T103) and filter (U1), is undertaken by following step:
(1) from the zinc ammoniacal liquor (S1) of dissolving workshop section in ammonia still (T101) after distillation is handled dense ammonia distillated by cat head, a part of first strong aqua (S3) advances tank used for storing ammonia behind condensation, separatory, thick ammonia (S4) enters ammonia recovery tower (T103), dense zinc liquid (S2) at the bottom of the tower enters in the filter (U1), 70 ~ 90 ℃ of temperature enter continuation processing recovery ammonia in the ammonia desorption tower (T102) through the filter zinc liquid (S5) after filter (U1) the filtered and recycled zinc oxide component; Wherein ammonia still (T101) top is tray column, and the bottom is the herringbone buffle-type tower, and charging is 70 ~ 125 ℃ of the top service temperatures of tower, working pressure 0 ~ 0.2MPa(A); The tray column form that ammonia still (T101) adopts can be bubbling class column plate, also can be the ejection-type column plate, and the herringbone baffle plate is single word veneer, double word baffle plate or many herringbones baffle plate; Filter is that flame filter press, whizzer, commentaries on classics are with vacuum filter or strip machine;
(2) contain part ammonia in the filter zinc liquid (S5), under the effect of alkali lye (S6), handle through ammonia desorption tower (T102), first tail gas (S9) emptying after condensation, cooling of cat head component, ammoniacal liquor (S8) advances tank used for storing ammonia, further utilize, waste water in the tower has reclaimed active principle after the desorption tower effect, purifying waste water at the bottom of the tower (S7) reached emission standard this moment, effluxes; Wherein ammonia desorption tower (T102) feed entrance point is the middle and upper part of tower, and the alkali lye import is on top or the middle part, 95 ~ 120 ℃ of service temperatures, working pressure 0 ~ 0.2MPa(A); Ammonia desorption tower (T102) can be the Mixed Design tower of tray column, packing tower or column plate and filler; Wherein filter contain ammonia in the zinc liquid (S5) concentration less than 2g/L, alkali lye (S6) is sodium hydroxide solution;
(3) from the thick ammonia (S4) of ammonia still (T101), under the effect of process water (S10) after ammonia recovery tower (T103) absorbs cat head tail gas concentration reduce greatly, second tail gas (S11) emptying, second strong aqua (S12) at the bottom of the tower advances tank used for storing ammonia and does further to utilize, the charging of process water (S10) cat head, air inlet at the bottom of thick ammonia (S4) tower; Ammonia recovery tower (T103) tower has stage casing circulation heat-obtaining device, 25 ~ 80 ℃ of service temperatures, working pressure 0 ~ 0.2MPa(A); Ammonia recovery tower (T103) is the Mixed Design tower of tray column, packing tower or column plate and filler, and stage casing circulation heat-obtaining device has one at least.
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| CN 201210001840 CN102515253B (en) | 2012-01-05 | 2012-01-05 | Production method for producing zinc oxide by ammonia process and comprehensively utilizing waste water |
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| CN 201210001840 CN102515253B (en) | 2012-01-05 | 2012-01-05 | Production method for producing zinc oxide by ammonia process and comprehensively utilizing waste water |
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| CN112408461B (en) * | 2020-12-10 | 2022-08-16 | 平江县吉成科技有限责任公司 | Preparation method of feed-grade active zinc oxide |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1210813A (en) * | 1998-07-24 | 1999-03-17 | 山西省稷山县福利化工厂 | Alkaline process for producing active zinc oxide |
| CN1267637A (en) * | 1999-03-20 | 2000-09-27 | 张铧 | Preparation of superfine active zinc oxide |
| US6555075B2 (en) * | 2001-05-23 | 2003-04-29 | Raymond Lee Nip | Method of preparing zinc carbonate |
| CN1944291A (en) * | 2006-10-17 | 2007-04-11 | 自贡鸿鹤化工股份有限公司 | Method for teating heavy alkali filter liquid in synthesizing alkali producing method |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1210813A (en) * | 1998-07-24 | 1999-03-17 | 山西省稷山县福利化工厂 | Alkaline process for producing active zinc oxide |
| CN1267637A (en) * | 1999-03-20 | 2000-09-27 | 张铧 | Preparation of superfine active zinc oxide |
| US6555075B2 (en) * | 2001-05-23 | 2003-04-29 | Raymond Lee Nip | Method of preparing zinc carbonate |
| CN1944291A (en) * | 2006-10-17 | 2007-04-11 | 自贡鸿鹤化工股份有限公司 | Method for teating heavy alkali filter liquid in synthesizing alkali producing method |
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Owner name: TIANJIN HAOYONG CHEMICAL ENGINEERING TECHNOLOGY CO Free format text: FORMER NAME: TIANJIN HAOYONG CHEMICAL TECHNOLOGY CO., LTD. |
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