CN101475194B - Method for recycling ammonia from low concentration ammonium chloride wastewater - Google Patents
Method for recycling ammonia from low concentration ammonium chloride wastewater Download PDFInfo
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- CN101475194B CN101475194B CN2009100210206A CN200910021020A CN101475194B CN 101475194 B CN101475194 B CN 101475194B CN 2009100210206 A CN2009100210206 A CN 2009100210206A CN 200910021020 A CN200910021020 A CN 200910021020A CN 101475194 B CN101475194 B CN 101475194B
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Abstract
The invention discloses a method for recovering ammonia from low-concentration ammonium chloride wastewater, which comprises the following steps that: an alkaline substance is added into the low-concentration ammonium chloride wastewater to prepare mixed slurry containing ammonia water and chloride salt; the mixed slurry is subjected to the separation and concentration of the ammonia water in an ammonia water distillation concentration tower to obtain ammonia vapor and a drained waste liquid; the ammonia vapor is conveyed to an ammonia water cooler for cooling treatment, and the ammonia water obtained by the cooling treatment is stored for standby; and the drained waste liquid is subjected to solid-liquid separation to obtain solid-phase residue and a waste liquid containing the chloride salt. The method evaporates the ammonia in the low-concentration ammonium chloride wastewater and concentrates the ammonia to an industrial grade concentration, and has the advantages of broad source of auxiliary materials, low cost, completely sealed technical process, and low energy consumption; and drained substances meet the requirement of no pollution and no nuisance.
Description
Technical field
The present invention relates to a kind of method that reclaims ammonia, especially relate to a kind of method that from low concentration ammonium chloride wastewater, reclaims ammonia.
Background technology
China is rare earth big country, and annual rare earth output is about 150,000 tons, and low concentration ammonium chloride wastewater is the particularly relief liquor that certainly leads to of rare-earth wet method separation industries of coloured industry.According to statistics, per minute from one ton of rare earth oxide mean consumption ammoniacal liquor or bicarbonate of ammonia more than 6 tons, and owing to be subjected to the limitation of production technique, and ammonium chloride content lower (its concentration mostly is 0.2-2.5mol/L greatly) in the waste discharge, only the ammonium chloride of the annual discharging of this rare-earth trade is above 1,000,000 tons.And synthetic 1,000,000 tons of ammonia need 80,000 ten thousand cubical Sweet natural gases, need about 300,000 tons of hard coals, therefore as in addition recycling of the ammonia in the waste water, can not cause the waste of resource.On the other hand, low concentration ammonium chloride wastewater can cause serious environmental to pollute.The generation rare-earth trade ammonia nitrogen waste water discharging of Ganzhou, Jiangsu in 2006 causes serious pollution incident to cause the Taihu Lake basin ammonia nitrogen to exceed standard, the area, packet header enters winter the Yellow River flow every year and reduces the ammonia nitrogen waste water severe overweight and cause severe contamination, caused that national environmental protection department pays much attention to, stood to make rare-earth trade rectify and improve.So the low-concentration ammonia-nitrogen Wastewater Recovery is utilized again becomes the important technology of a present puzzlement rare-earth trade difficult problem.
The present low-concentration ammonia-nitrogen wastewater recycling process that generally adopts, be mainly direct concentration and evaporation crystallization and reclaim ammonium chloride, or ammonium chloride adds circulation agent evaporation recovery hydrochloric acid and ammoniacal liquor, the former has following shortcoming: the rate of recovery is too low and the heat energy consumption is big, ammonium chloride market saturation in addition, a large amount of ammonium chloride is piled up pin and is not fallen, and a lot of enterprises Halfway Stopping of having to reclaims and produces; The latter produces the ammoniacal liquor obtain and concentration of hydrochloric acid is too low can't use, and energy consumption is big, so can't form suitability for industrialized production.
Summary of the invention
Technical problem to be solved by this invention is at above-mentioned deficiency of the prior art, a kind of method that reclaims ammonia from low concentration ammonium chloride wastewater is provided, with the ammonia in low concentration ammonium chloride wastewater evaporation and be concentrated to technical grade concentration, auxiliary material wide material sources and cost are low, technological process seals fully, energy consumption is low, and discharge meets pollution-free non-harmful requirement.
For solving the problems of the technologies described above, the technical solution used in the present invention is:. a kind of method that reclaims ammonia from low concentration ammonium chloride wastewater is characterized in that this method may further comprise the steps:
(1) hybrid reaction technology: in low concentration ammonium chloride wastewater, add alkaline matter, stir ammonium chloride and alkaline matter are fully reacted, obtain containing the mixed slurry of ammoniacal liquor and chloride salt, described low concentration ammonium chloride wastewater is meant that concentration is the ammonium chloride waste-water of 0.2-2.5mol/L;
(2) ammonia separates concentration technology: the mixed slurry in the step (1) is transported to the separation of carrying out ammoniacal liquor in the ammonia distillation upgrading tower and concentrates with anti-wear mortar pump, obtain ammonia steam and discharging waste liquid;
(3) cool back the skill of knocking off: the ammonia delivery of steam in the step (2) is carried out cooling process in the ammoniacal liquor water cooler, and the ammoniacal liquor that obtains after the cooling process is left in the ammoniacal liquor hold-up vessel;
(4) discharging process for treating waste liquor: the discharging waste liquid in the step (2) is carried out solid-liquid separation, obtain the waste liquid of solid phase slag and chloride salt, and with solid phase slag and discharging of waste liquid or utilization again.
Between step (1) and step (2), also comprise,, remove the particulate matter impurity in the mixed slurry the sedimentation in multistage continuous natural subsidence groove of the mixed slurry in the step (1).
In the inside of ammonia distillation upgrading tower described in the step (2), by adjusting the feed rate and the steam rates of mixed slurry, make the tower top temperature of ammonia distillation upgrading tower remain on 80 ℃-98 ℃, water vapor pressure remains on 1MPa-6MPa.
The tower top temperature of described ammonia distillation upgrading tower remains on 85 ℃-98 ℃.
The temperature of cooling water of ammoniacal liquor water cooler described in the step (3) remains on 15 ℃-40 ℃.
Described alkaline matter is a sodium hydroxide solution, and in the sodium hydroxide solution in sodium hydroxide and the low concentration ammonium chloride wastewater weight ratio of ammonium chloride be 1: 1.3-1.6.
Described alkaline matter is a calcium carbide cream, and the weight ratio of ammonium chloride is 1 in calcium carbide cream and the low concentration ammonium chloride wastewater: 1-1.5.
Described alkaline matter is a unslaked lime, and the weight ratio of ammonium chloride is 1 in unslaked lime and the low concentration ammonium chloride wastewater: 0.5-1.
The present invention compared with prior art has the following advantages:
1, the present invention has realized the ammonia recovery of resources, and raw materials cost is low.Raw material of the present invention is that rare-earth wet method separates or the concentration of coloured industry discharging is the low concentration ammonium chloride wastewater of 0.2-2.5mol/L, when realizing the recycling of ammonia resource, has solved low concentration ammonium chloride wastewater and has directly discharged the pollution problem that causes.Auxiliary material among the present invention is an alkaline matter, gathers materials on the spot as the case may be or refuse reclamation, as calcium carbide cream, unslaked lime, sodium hydroxide solution, white lime, basic magnesium chloride or other alkaline matters.The calcium carbide cream that with the main component is calcium hydroxide, moisture and small amount of carbon is example, and calcium carbide cream is produced the chemical spent material of calcium carbide as chemical industry, and its cost is low, obtains easily, and meets the environmental requirement of refuse reclamation.
2, the ammonia concn height that utilizes the present invention to obtain, other discharges that obtain simultaneously meet environmental emission standard, and recyclable utilization again.The experiment proved that the ammoniacal liquor volumetric molar concentration of utilizing this recovery method to obtain is 8-15mol/L, reaches industrial application target, the volumetric molar concentration of ammonia only is 0.1-0.005mol/L in the discharging waste liquid that obtains simultaneously.On the other hand, the pH value of solid phase slag meets the environmental emission standard requirement fully less than 9 in the discharging waste liquid; And the solid phase slag discharges or recovery re-uses as cement raw material, and discharging of waste liquid or recovery re-use the deep processing of making corresponding salt.
3, the main equipment that adopts is ammonia distillation upgrading tower and ammoniacal liquor water cooler among the present invention, technological process is simple, produce environment friendly and pollution-free, and energy expenditure is low, especially this ammonia distillation upgrading tower is once with the ammonia in mixed slurry evaporation and be concentrated to technical grade concentration, 80% of institute's energy consumption acts on the strong aqua that obtains, and reclaims the energy consumption of evaporation fully of technology well below tradition.
Below by drawings and Examples, technical scheme of the present invention is described in further detail.
Description of drawings
Fig. 1 is the structural representation of ammonia distillation upgrading tower of the present invention.
Description of reference numerals:
1-ammonia vapour outlet; The 2-Despumation device; The 3-liquor inlet;
The 4-riser; 5-shelves stream plate; The 6-tower body;
The 7-manhole; Liquid pipe under the 8-; The 9-twin-stage concentrates cover;
The 10-steam inlet; 11-discharges waste liquid outlet; The 12-column plate.
Embodiment
A kind of method that reclaims ammonia from low concentration ammonium chloride wastewater of the present invention may further comprise the steps:
(1) hybrid reaction technology: is concentration that the low concentration ammonium chloride wastewater of 0.2-2.5mol/L is transported in the steel basin, in low concentration ammonium chloride wastewater, add alkaline matter, and stir, after ammonium chloride and alkaline matter fully react, obtain containing the mixed slurry of ammoniacal liquor and chloride salt, described mixed slurry is the mixture of pasty state or suspension.Described alkaline matter is gathered materials on the spot or refuse reclamation according to local particular case, as calcium carbide cream, unslaked lime, sodium hydroxide solution, white lime, basic magnesium chloride or other alkaline matters.
(2) ammonia separates concentration technology: the mixed slurry in the step (1) is transported to the separation of carrying out ammoniacal liquor in the ammonia distillation upgrading tower and concentrates with anti-wear mortar pump, obtain ammonia steam and discharging waste liquid.
Wherein, as shown in Figure 1, described ammonia distillation upgrading tower comprises that inside is provided with the tower body 6 of multilayer column plate 12, column plate 12 is provided with twin-stage and concentrates cover 9, riser 4 and shelves stream plate 5, and two-layer up and down column plate 12 communicates by following liquid pipe 8, the top that is positioned at tower body 6 is provided with ammonia vapour outlet 1 and Despumation device 2, the upper portion side wall of tower body 6 is provided with liquor inlet 3, the bottom sidewall of tower body 6 is provided with steam inlet 10 and discharging waste liquid outlet 11, is provided with a plurality of manholes 7 on the tower body 6 between liquor inlet 3 and steam inlet 10.In the production, according to containing ammonia concentration in the low concentration ammonium chloride wastewater of concrete use, the height of tower body 6 is 8 meters---20 meters, it is 6 grades-15 grades that the number of plies of column plate 12 is promptly distilled progression.
With anti-wear mortar pump the mixed slurry that obtains in the step (1) is transported in the ammonia distillation upgrading tower by liquor inlet 3, and from ammonia vapour outlet 1 fluming water steam, finally obtain ammonia steam and discharging waste liquid, wherein, ammonia steam escapes and enter step (3) from ammonia vapour outlet 1 from ammonia vapour outlet 1, the discharging waste liquid escapes and enter step (4) from discharging waste liquid outlet 11.
In the ammonia distillation upgrading tower, by adjusting the feed rate and the steam rates of mixed slurry, make the tower top temperature of ammonia distillation upgrading tower remain on 80 ℃-98 ℃, water vapor pressure keeps 1MPa-6MPa, wherein, facts have proved that through industrialization when the tower top temperature of ammonia distillation upgrading tower remained on 85 ℃-98 ℃, the volumetric molar concentration of ammonia only was 0.1-0.005mol/L in the discharging waste liquid.
(3) cool back the skill of knocking off: the ammonia delivery of steam that obtains in the step (2) is carried out cooling process in the ammoniacal liquor water cooler, and leave in the ammoniacal liquor hold-up vessel ammoniacal liquor that obtains after the cooling process standby.Wherein, the ammoniacal liquor water cooler is plain carbon stool or stainless steel, and the heat interchanging area of this water cooler is selected 20-200 square metre for use according to the difference of output, and its water coolant is selected tap water for use, and the temperature of water coolant remains on 15 ℃-40 ℃ in process of cooling.
(4) discharging process for treating waste liquor: the discharging waste liquid in the step (2) is carried out solid-liquid separation, obtain the waste liquid of solid phase slag and chloride salt, and with solid phase slag and discharging of waste liquid or utilization again.Wherein, solid-liquid separating equipment can be the barrier film plate-and-frame filter press of band washing, also can be the solid-liquid separating equipment of other band washing, facts have proved that through industrialization the solid phase slag pH value that obtains after the solid-liquid separation meets the environmental emission standard requirement fully less than 9.The solid phase slag discharges or recovery re-uses as cement raw material, and discharging of waste liquid or recovery re-use the deep processing of making corresponding salt.
Among the present invention as when using calcium carbide cream, unslaked lime, white lime or basic magnesium chloride etc. to contain the more alkaline matter of granule foreign, between step (1) and step (2), also comprise, with the sedimentation in multistage continuous natural subsidence groove of the mixed slurry in the step (1), after removing the particulate matter impurity in the mixed slurry, mixed slurry is entering step (2); Regularly the particulate matter in the multistage continuous natural subsidence groove is dragged in another filter vat, discharge with water wash and after filter is done naturally.
Embodiment one:
Alkaline matter is selected sodium hydroxide solution for use, in the sodium hydroxide solution in sodium hydroxide and the low concentration ammonium chloride wastewater weight ratio of ammonium chloride be 1: 1.3-1.6, the ammonia that carries out hybrid reaction technology, the step (2) of step (1) as mentioned above successively separates the knock off discharging process for treating waste liquor of skill and step (4) of cooling back of concentration technology, step (3), finally obtains ammoniacal liquor.
Embodiment two:
Alkaline matter is selected calcium carbide cream for use, and the weight ratio of ammonium chloride is 1 in calcium carbide cream and the low concentration ammonium chloride wastewater: 1-1.5, carry out the hybrid reaction technology of step (1) as mentioned above, behind the mixed slurry sedimentation removal particulate matter impurity that obtains in the step (1), the ammonia that enters step (2) more successively separates concentration technology, the discharging process for treating waste liquor that cools back knock off skill and step (4) of step (3) finally obtains ammoniacal liquor.
Embodiment three:
Alkaline matter is selected unslaked lime for use, and the weight ratio of ammonium chloride is 1 in unslaked lime and the low concentration ammonium chloride wastewater: 0.5-1, carry out the hybrid reaction technology of step (1) as mentioned above, behind the mixed slurry sedimentation removal particulate matter impurity that obtains in the step (1), the ammonia that enters step (2) more successively separates concentration technology, the discharging process for treating waste liquor that cools back knock off skill and step (4) of step (3) finally obtains ammoniacal liquor.
The above; it only is preferred embodiment of the present invention; be not that the present invention is imposed any restrictions, every according to the technology of the present invention essence to any simple modification, change and equivalent structure transformation that above embodiment did, all still belong in the protection domain of technical solution of the present invention.
Claims (6)
1. method that reclaims ammonia from low concentration ammonium chloride wastewater is characterized in that this method may further comprise the steps:
(1) hybrid reaction technology: in low concentration ammonium chloride wastewater, add alkaline matter, stir ammonium chloride and alkaline matter are fully reacted, obtain containing the mixed slurry of ammoniacal liquor and chloride salt, described low concentration ammonium chloride wastewater is meant that concentration is the ammonium chloride waste-water of 0.2-2.5mol/L;
(2) ammonia separates concentration technology: the mixed slurry in the step (1) is transported to the separation of carrying out ammoniacal liquor in the ammonia distillation upgrading tower and concentrates with anti-wear mortar pump, obtain ammonia steam and discharging waste liquid; In the inside of described ammonia distillation upgrading tower, by adjusting the feed rate and the steam rates of mixed slurry, make the tower top temperature of ammonia distillation upgrading tower remain on 85 ℃-98 ℃, water vapor pressure remains on 1MPa-6MPa; Described ammonia distillation upgrading tower comprises that inside is provided with the tower body of multilayer column plate, column plate is provided with twin-stage and concentrates cover, riser and shelves stream plate, and two-layer up and down column plate communicates by following liquid pipe, the top that is positioned at tower body is provided with ammonia vapour outlet and Despumation device, the upper portion side wall of tower body is provided with liquor inlet, the bottom sidewall of tower body is provided with steam inlet and discharging waste liquid outlet, is provided with a plurality of manholes on the tower body between liquor inlet and steam inlet;
(3) cool back the skill of knocking off: the ammonia delivery of steam in the step (2) is carried out cooling process in the ammoniacal liquor water cooler, and the ammoniacal liquor that obtains after the cooling process is left in the ammoniacal liquor hold-up vessel;
(4) discharging process for treating waste liquor: the discharging waste liquid in the step (2) is carried out solid-liquid separation, obtain the waste liquid of solid phase slag and chloride salt, and with solid phase slag and discharging of waste liquid or utilization again.
2. according to the described a kind of method that from low concentration ammonium chloride wastewater, reclaims ammonia of claim 1, it is characterized in that: between step (1) and step (2), also comprise, with the sedimentation in multistage continuous natural subsidence groove of the mixed slurry in the step (1), remove the particulate matter impurity in the mixed slurry.
3. according to claim 1 or 2 described a kind of methods that reclaim ammonia from low concentration ammonium chloride wastewater, it is characterized in that: the temperature of cooling water of ammoniacal liquor water cooler described in the step (3) remains on 15 ℃-40 ℃.
4. according to the described a kind of method that from low concentration ammonium chloride wastewater, reclaims ammonia of claim 1, it is characterized in that: described alkaline matter is a sodium hydroxide solution, and in the sodium hydroxide solution in sodium hydroxide and the low concentration ammonium chloride wastewater weight ratio of ammonium chloride be 1: 1.3-1.6.
5. according to the described a kind of method that reclaims ammonia from low concentration ammonium chloride wastewater of claim 2, it is characterized in that: described alkaline matter is a calcium carbide cream, and the weight ratio of ammonium chloride is 1 in calcium carbide cream and the low concentration ammonium chloride wastewater: 1-1.5.
6. according to the described a kind of method that reclaims ammonia from low concentration ammonium chloride wastewater of claim 2, it is characterized in that: described alkaline matter is a unslaked lime, and the weight ratio of ammonium chloride is 1 in unslaked lime and the low concentration ammonium chloride wastewater: 0.5-1.
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| CN2009100210206A CN101475194B (en) | 2009-01-22 | 2009-01-22 | Method for recycling ammonia from low concentration ammonium chloride wastewater |
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| CN101941719B (en) * | 2010-05-25 | 2012-05-23 | 河北科技大学 | Method for combined production of ammonia and basic calcium chloride by decomposing ammonium chloride |
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| CN103043823A (en) * | 2012-12-28 | 2013-04-17 | 浙江闰土股份有限公司 | Method for recycling waste water containing ammonium chloride |
| CN103755002A (en) * | 2014-01-21 | 2014-04-30 | 江苏隆昌化工有限公司 | Method of recycling ammonium chloride |
| CN105417823A (en) * | 2015-12-25 | 2016-03-23 | 周振喜 | Method of recycling ammonia from low-concentration ammonium chloride waste water |
| CN108314112B (en) * | 2017-01-17 | 2020-08-21 | 中国石油化工股份有限公司 | Method for treating waste water containing ammonium salt |
| CN108314115B (en) * | 2017-01-17 | 2020-08-21 | 中国石油化工股份有限公司 | Method for treating waste water containing ammonium salt |
| NL2020788B1 (en) | 2017-04-21 | 2019-06-26 | China Petroleum & Chem Corp | Apparatus and Method for Treating Waste Water Containing Ammonium Salts |
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| CN108715496B (en) * | 2018-06-07 | 2019-03-22 | 全南县新资源稀土有限责任公司 | A method of recycling ammonia from Rare Earth Separation waste liquid |
| CN108467049B (en) * | 2018-06-07 | 2023-07-25 | 全南县新资源稀土有限责任公司 | System for retrieve ammonia in follow tombarthite separation waste liquid |
| CN110104660B (en) * | 2019-05-17 | 2021-09-03 | 大连科汇工程技术有限公司 | System and process for separating chlorine in ammonia-containing gas by cooling and stripping |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85101146A (en) * | 1985-04-01 | 1987-01-17 | 三菱金属株式会社 | Processing contains the method for ammonium and fluorium ion liquid |
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2009
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85101146A (en) * | 1985-04-01 | 1987-01-17 | 三菱金属株式会社 | Processing contains the method for ammonium and fluorium ion liquid |
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Assignee: Qunan New Resources Rare Earth Co., Ltd. Assignor: Xi'an Xijun New Material Co., Ltd. Contract record no.: 2011610000029 Denomination of invention: Method for recycling ammonia from low concentration ammonium chloride wastewater Granted publication date: 20101229 License type: Common License Open date: 20090708 Record date: 20110607 |
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Effective date of registration: 20160720 Address after: Hexi Industrial Zone 014010 the Inner Mongolia Autonomous Region Baotou City 01 street 777888 Queensland smelter Patentee after: Baotou West Environmental Protection Technology Co., Ltd. Address before: 710086 box twenty-ninth, Kunming Road, Shaanxi, Xi'an Patentee before: Xi'an Xijun New Material Co., Ltd. |
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Address after: Hexi Industrial Zone 014010 the Inner Mongolia Autonomous Region Baotou City 01 street 777888 Queensland smelter Patentee after: Baotou West Environmental Protection Technology Co., Ltd. Address before: Hexi Industrial Zone 014010 the Inner Mongolia Autonomous Region Baotou City 01 street 777888 Queensland smelter Patentee before: Baotou West Environmental Protection Technology Co., Ltd. |