CN202671209U - Mother liquor ammonia neutralization device for nitric phosphate production - Google Patents
Mother liquor ammonia neutralization device for nitric phosphate production Download PDFInfo
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- CN202671209U CN202671209U CN 201220320544 CN201220320544U CN202671209U CN 202671209 U CN202671209 U CN 202671209U CN 201220320544 CN201220320544 CN 201220320544 CN 201220320544 U CN201220320544 U CN 201220320544U CN 202671209 U CN202671209 U CN 202671209U
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Abstract
The utility model discloses a mother liquor ammonia neutralization device for nitric phosphate production. The mother liquor ammonia neutralization device comprises a first-section neutralization device, a second-section neutralization device and a neutralization tail gas washing device, wherein the second-section neutralization device is a forced circulation tubular reactor, and a flash separation chamber, a descending tube, a circulating pump and a reaction tube are sequentially communicated to form a reaction system with an annular closed structure. Therefore, the phenomena of high viscosity of mother liquor ammonia neutralization slurry, material adhesion and scabbing in the nitric phosphate production process are eliminated. The second-section neutralization device has a multi-point charging structure and is used for forced circulation tubular reaction, a viscous area in the neutralization process is avoided, materials can be uniformly mixed, slurry is high in flowability, and ammonia (NH3) is low in loss.
Description
Technical field
The utility model is relevant with a kind of mother liquor ammonia neutralising arrangement of producing nitrophosphate fertilizer, in particular for produce the mother liquor ammonia neutralising arrangement of a kind of nitrophosphate fertilizer of nitrophosphate fertilizer as the raw material cold method take nitric acid and phosphorus ore.
Background technology
China Tianji Coal Chemical Industry Group Co., Ltd. Nitro Phosphate Unit is to introduce from Norway the eighties, and the modernized large production equipment of 900,000 tons of nitrophosphate fertilizers is produced in design per year, adopts indirect refrigeration deliming and double-shaft horizontal granulation patent production technology.The production unit that production process cooperates comprises: converting apparatus of thickening equipment, granulation, drying, screening, packing and the nitrocalcite of the nitric acid resolving device of phosphorus ore, acid non-soluble substance separating device, nitrocalcite Crystallization Separation equipment, mother liquor ammonia neutralizing device, NP slip etc., wherein, nitrophosphate fertilizer mother liquor ammonia neutralizing device is one of main production equipments, adopt in the normal pressure and groove type reactor, in minutes three sections and structure.
Cold method can only be isolated in the acidolysis slip 75% of total calcium except crystallization nitrocalcite technique equipment used, therefore, and in the N-process of Nitro Phosphate Unit, because the phosphoric acid mother liquor contains higher Ca
2+Mg with trace
2+, Fe
3+, Al
3+Reach the impurity such as acid non-soluble substance, in the neutralising arrangement process, can form complicated compound, they are gelatinous tiny xln, thereby increase with phosphoric acid in causing, especially in and the pH value reach 2.7 and at 4.5 o'clock, phosphoric acid will the value of peaking, cause ramming material in neutralizing device, to occur and the phenomenon that scabs so that in and technique and equipment thereof can't operate.For this reason, in avoiding and the viscosity peak value, in the Nitro Phosphate Unit mother liquor ammonia and operation be designed to three sections ambient neutral process, acid divides three sections to finish with the neutralization reaction of ammonia, each section neutralizing device control pH value is 1.6-2.0,2.8-3.2,5.6-6.0.
Normal pressure neutralizing device Main Problems is that the pH value is restive, ammonification, slip thickness phenomenon occur easily, and ammonia effusion loss is larger, and air bleeds more, and ramming material appears in the neutralizing well top, the phenomenon that scabs, severe operational environment.
The mother liquor ammonia neutralizing device of GSFC of Gujarat, India nation (GNFC) nitrophosphate fertilizer is divided into two sections neutralizing devices, and one section neutralizing device adopts the pump circulation pipeline reactor, passes into 80% of total ammonia amount at this, and pH is controlled at 2.5-3.2; Two sections neutralizing devices adopt the normal pressure groove type reactor, pass into 20% of total ammonia amount at this, and pH is controlled at 5.5.This device is reasonable in design, the pump circulation reaction unit is adopted in one section neutralization, has fully guaranteed the maximum absorption of ammonia, and two sections neutralizing devices only need pass into 20% of total ammonia amount, in having avoided occuring in normal pressure reactor and vigorous reaction, the ammonia of whole system is also overflowed less.
Sichuan University's clock basis and seminar adopt " enriching slurry method " to set up wet method ammonium phosphate production process and the equipment thereof of grade phosphorus mine characteristics in suitable China.Chinese patent CN 100371238C adopts method and the secondary ammoniation reactor of the concentrated production diammonium phosphate of acid slime that good reference also is provided.
Summary of the invention
The technical problems to be solved in the utility model is to produce in the nitrophosphate fertilizer mother liquor ammonia and technique according to existing, and design is applied in this and the neutralising arrangement of technique, and selects suitable feeding raw materials from more than one places position.Ambient neutral process is to contain higher Ca at present
2+Mg with trace
2+, Fe
3+, Al
3+And the acid slime of acid non-soluble substance carries out the ammonia neutralization, during can causing, reaction generation gel crystals increases with phosphoric acid, and adopt normal pressure neutralizing device pH value restive, ammonification appearred easily, ammonia is overflowed and to be bled manyly with air, especially reaches 2.7 and at 4.5 o'clock in the pH value, and phosphoric acid peaks, ramming material and the phenomenon that scabs very easily appear in equipment so that in and technique and operation of equipment thereof can't carry out.To this, provide a kind of mother liquor ammonia neutralising arrangement of producing nitrophosphate fertilizer.
The utility model addresses the above problem a kind of technical scheme of producing the neutralising arrangement of nitrophosphate fertilizer mother liquor ammonia of taking, comprise one section neutralising arrangement, two sections neutralising arrangements and in and the washing tail gas device; Its described neutralising arrangement is to carry out the ammonia neutralization for the phosphoric acid mother liquor of Phosphate Fertilizer Production process decomposing phosphorite by using nitric acid gained being removed nitrocalcite total amount 75%, what its described two sections neutralising arrangements produced contains ammonia gas by one section neutralising arrangement of pipeline input, then import smoke stack emission with the washing tail gas device in the tail gas warp of one section neutralising arrangement generation, in and the washings of washing tail gas device return two sections neutralising arrangements by pipeline, consist of nitrophosphate fertilizer mother liquor ammonia neutralising arrangement; Wherein:
Described two sections neutralising arrangements are pump circulation tubular reactors, are the reaction systems that is communicated with successively the looping enclosed construction by flash separation chamber, downtake, recycle pump and reaction tubes;
Described flash separation chamber is that inner wall surface thereof is provided with flash separation chamber baffle plate, top is provided with slip and adds entrance, bottom and be provided with the circulation slip and add mouthful, the middle part is provided with the slurry outlet liquid sealing pipe of slurry outlet and connection thereof, top ends is installed on scum dredger and contains the ammonia gas outlet, and the bottom is communicated with downtake;
Be communicated with successively on the described downtake be provided with in and tail gas washing liquid entrance, ammonium nitrate slip add in entrance and one section and slip entrance I;
Be communicated with successively on the described reaction tubes and be provided with in the gas ammonia entrance I, one section and slip entrance II and gas ammonia entrance II.
In the technical scheme of above-mentioned neutralising arrangement, further additional technical feature is: the reinforced distance setting of described two sections neutralising arrangement gas ammonia entrance I and gas ammonia entrance II is 1-3m; Be provided with the downtake baffle plate on the inner-wall surface of described two sections neutralising arrangement downtakes, and in laying respectively at and tail gas washing liquid entrance, ammonium nitrate slip add in entrance and one section and in the upstream canal of slip entrance I entrance; Be provided with the reaction tubes baffle plate on the inner-wall surface of described two sections neutralising arrangement reaction tubess, and lay respectively in the gas ammonia entrance I, one section and slip entrance II and gas ammonia entrance II entrance upstream canal in; The angle that axially arranges of described downtake baffle plate and reaction tubes baffle plate is 93
0～160
0Between; Described two sections neutralising arrangement slurry outlets are that it is higher than 1 meter that the circulation slip adds mouth, and are positioned under the slip entrance.
Realize the above-mentioned a kind of technical scheme of producing nitrophosphate fertilizer mother liquor ammonia neutralising arrangement of the utility model, compared with prior art, its advantage and positively effect are as follows:
Two sections neutralising arrangements adopt the pump circulation tubular reactor, in effectively having avoided and thickness point pH=2.7 and 4.5, the feeding raw materials from more than one places position further is set, effectively prevent the local ammonification of crossing, both reduced the process recycle ratio, saved energy, improved again the assimilated efficiency of ammonia, also keep simultaneously the stationarity of process pH, avoided bleeding of normal pressure reactor air, especially reduced in the chimney drainage rate of ammonia and the quantity discharged of tail gas thereof.
In the upstream line of the gas ammonia entrance of downtake and reaction tubes and slip entrance, add respectively downtake baffle plate and reaction tubes baffle plate, the one, be conducive to import gas ammonia, the 2nd, be conducive to gas ammonia and mix with the effective of reaction slurry, improved simultaneously the less turbulence of fluid, prevented slip the ramming material in reaction tubes, scab and stop up.
Two sections neutralising arrangements arrange slip adding before the equipment operation of pH=5.6-6.0, have guaranteed that the circulation slip has good flowability, have improved stability of system in the equipment running process.
On downtake, arrange before the recycle pump ammonium nitrate solution and in and tail gas washing liquid add entrance, adjusting reaction slurry N/P
2O
5In the time of ratio, improve the less turbulence of fluid, and effectively reduced the viscosity of reaction slurry, and be conducive to prevent from reacting the local ammonification phenomenon of crossing of too fast appearance.
Nitric acid, phosphoric acid and ammonia react are produced a large amount of reaction heat, be used for the moisture of the gentle material slurry of reacting by heating slip, per kilogram ammonia evaporates 1.3 kg of water approximately, the process energy conservation successful, even can save the preheater of slip evaporation; Adopt pump circulation tubular reactor feeding raw materials from more than one places, the ammonia loss is few, purify by one section neutralization reaction groove with tail gas in two sections, in one section and tail gas enter in and the tail gas washing tower absorption condensation, then through smoke stack emission, this structure setting not only can reduce the quantity discharged of multiple fertile chimney water vapor, and has kept the water balance of apparatus system, and the process environment protecting also clearly.
The slurry outlet that flash separator is set is higher than circulation slip entrance, has improved the temperature of reaction mass, has further reduced slip and has got viscosity, has prevented separating out of crystallization.
Be provided with liquid sealing pipe at the slurry outlet pipeline, guarantee that forced circulation device is in complete sealed state, can prevent the suck-back of air, can reduce again the effusion rate of gas ammonia.
Description of drawings
Fig. 1 is the utility model for the production of in the nitrophosphate fertilizer mother liquor ammonia and two sections neutralising arrangement structural representations of the neutralising arrangement of technique.
Fig. 2 is the local structure synoptic diagram of the utility model Fig. 1 downtake.
Fig. 3 is the local structure synoptic diagram of the utility model Fig. 1 reaction tubes.
Among the figure: 1: the flash separation chamber; 2: flash separation chamber baffle plate; 3: the slip entrance; 4: scum dredger; 5: contain the ammonia gas outlet; 6: slurry outlet; 7: liquid sealing pipe; 8: downtake; 9: in and the tail gas washing liquid entrance; 10: ammonium nitrate slip entrance; In 11: one sections and slip entrance I; 12: recycle pump; 13: gas ammonia entrance I; 14: reaction tubes; In 15: one sections and slip entrance II; 16: gas ammonia entrance II; 17: circulation slip entrance; 18: the downtake baffle plate; 19: the reaction tubes baffle plate.
Embodiment
Below in conjunction with accompanying drawing embodiment of the present utility model is made an explanation, but content of the present utility model not only is confined to the scope of cited embodiment.
The utility model is on existing basis for the production of nitrophosphate fertilizer mother liquor ammonia neutralising arrangement, in conjunction with China's phosphorus ore characteristics, from the material essential attribute, nitrophosphate fertilizer mother liquor ammonia neutralising arrangement has been done further improvement, and for the existing deficiency of neutralising arrangement, select suitable feeding raw materials from more than one places point, so that N-process can be under the pH Value Operations situation than high stable, successfully avoid slip thickness district, process pH value is easy to control, is not easy to occur ammonification, and ammonia is overflowed and bled few with air, equipment ramming material and the phenomenon that scabs are few, a kind of mother liquor ammonia neutralising arrangement for the production of nitrophosphate fertilizer that for this reason provides.
As described in Fig. 1～Fig. 3, implement a kind of mother liquor ammonia neutralising arrangement of producing nitrophosphate fertilizer of the utility model, comprise one section neutralising arrangement, two sections neutralising arrangements and in and the washing tail gas device; Its described neutralising arrangement is to neutralize for the phosphoric acid mother liquor ammonia of removing nitrocalcite total amount 75% to producing the decomposing phosphorite by using nitric acid gained; What its described two sections neutralising arrangements produced contains ammonia gas by one section neutralising arrangement of pipeline input, the tail gas that one section neutralising arrangement produces through in and the washing tail gas device, rear importing smoke stack emission, in and the washings of washing tail gas device turn back to two sections neutralising arrangements through pipeline, consist of nitrophosphate fertilizer mother liquor ammonia neutralising arrangement with this; Wherein:
Implement two sections neutralising arrangements, comprise a pump circulation tubular reactor, this pump circulation tubular reactor is to be communicated with successively looping enclosed construction system by flash separation chamber 1, downtake 8, recycle pump 12, reaction tubes 14.Wherein:
The inner-wall surface of flash separation chamber 1 is provided with flash separation chamber baffle plate 2, the top is provided with scum dredger 4 and contains ammonia gas outlet 5, slurry outlet 6 and slurry outlet liquid sealing pipe 7 thereof are arranged at the middle and upper part of flash separation chamber 1, the slip of pH=5.6-6.0 adds entrance 3 and the circulation slip adds the up and down position that mouth 17 is arranged at flash separation chamber 1, the bottom of flash separation chamber 1 is communicated with downtake 8, and on downtake 8, be communicated with successively be provided with in and tail gas washing liquid entrance 9, the ammonium nitrate slip adds in entrance 10 and one section and slip entrance I 11, postposition is communicated with recycle pump 12, the reaction tubes 14 that is communicated with behind the recycle pump 12, and be disposed with gas ammonia entrance I 13 on the reaction tubes 14, in one section and slip entrance II 15 and gas ammonia entrance II 16.
In the technical scheme of two sections neutralising arrangements of above-mentioned enforcement, especially additional technical characterictic is:
The one, be provided with in one section of 50% the acid slime and slip entrance I 11 on the top of downtake 8; Be provided with the gas ammonia entrance II 16 that adds the required gas ammonia total amount 15% of neutralization on the top of reaction tubes 14, be provided with in one section of 50% the acid slime and slip entrance II 15 in the middle and upper part of reaction tubes 14, the bottom is provided with 35% the gas ammonia entrance I 13 that adds the required gas ammonia total amount of neutralization.
The 2nd, gas ammonia entrance I 13 arranges apart from being 1-3m with the neutralization of gas ammonia entrance II 16 is reinforced, and it is better that 3m especially is set.
The 3rd, gas ammonia entrance I 13, gas ammonia entrance II 16, in and tail gas washing liquid entrance 9, ammonium nitrate slip add in entrance 10 and one section and in the downstream canal of slip entrance I 11 entrances and be respectively arranged with a downtake baffle plate 18 and a reaction tubes baffle plate 19.
Described downtake baffle plate 18 with the angle that axially arranges of reaction tubes baffle plate 19 is: 93
0～160
0Between.
Above-mentioned downtake baffle plate 18 reaction tubes baffle plates 19 are at each feeding mouth one baffle plate to be set, and realize that its material that enters fully mixes with ducted material.
The 4th, the setting of slurry outlet 6 is to be higher than the 1m place that the circulation slip adds mouth 17, is positioned under the slip entrance 3.
Five is that one section neutralising arrangement is a synthesis under normal pressure groove, for the preparation of the acid slime of pH=1.6-2.0.
Six is that two sections neutralising arrangements are pump circulation tubular reactors, for the preparation of the acid slime of pH=5.6-6.0.Its process conditions is little negative pressure 100Pa (vacuum tightness), and temperature of reaction is controlled to be 125-135 ℃, and the pulp flow speed control is made as 1-3m/s, and the circulation multiple is controlled to be 30-50, and cycle index is set to 12-15/h, quality percentage composition 10-15%.
The above-mentioned a kind of mother liquor ammonia neutralising arrangement of producing nitrophosphate fertilizer implemented of the utility model, it arranges plate washer in flash separation chamber 1, downtake 8 and reaction tubes 14 all be fully to mix in limited room and time for the material that will enter, those skilled in the art knows and should how to arrange and set number, needn't make more detailed specifying here.
Claims (6)
1. mother liquor ammonia neutralising arrangement of producing nitrophosphate fertilizer, comprise one section neutralising arrangement, two sections neutralising arrangements and in and the washing tail gas device; Its described neutralising arrangement is to carry out the ammonia neutralization for the phosphoric acid mother liquor of Phosphate Fertilizer Production process decomposing phosphorite by using nitric acid gained being removed nitrocalcite total amount 75%, what its described two sections neutralising arrangements produced contains ammonia gas by one section neutralising arrangement of pipeline input, then import smoke stack emission with the washing tail gas device in the tail gas warp of one section neutralising arrangement generation, in and the washings of washing tail gas device return two sections neutralising arrangements by pipeline, consist of nitrophosphate fertilizer mother liquor ammonia neutralising arrangement; Wherein:
Described two sections neutralising arrangements are pump circulation tubular reactors, are the reaction systems that is communicated with successively the looping enclosed construction by flash separation chamber (1), downtake (8), recycle pump (12) and reaction tubes (14);
Described flash separation chamber (1) is that inner wall surface thereof is provided with flash separation chamber baffle plate (2), top is provided with slip and adds entrance (3), bottom and be provided with the circulation slip and add mouthful (17), the slurry outlet liquid sealing pipe (7) that the middle part is provided with slurry outlet (6) and is communicated with, top ends is installed on scum dredger (4) and contains ammonia gas outlet (5), and the bottom is communicated with downtake (8);
Be communicated with successively on the described downtake (8) be provided with in and tail gas washing liquid entrance (9), ammonium nitrate slip add in entrance (10) and one section and slip entrance I (11);
Be communicated with successively on the described reaction tubes (14) and be provided with in the gas ammonia entrance I (13), one section and slip entrance II (15) and gas ammonia entrance II (16).
2. neutralising arrangement as claimed in claim 1, its described two sections neutralising arrangement gas ammonia entrance I (13) are 1-3m with the reinforced distance setting of gas ammonia entrance II (16).
3. neutralising arrangement as claimed in claim 1, be provided with a downtake baffle plate (18) on the inner-wall surface of its described two sections neutralising arrangement downtakes (8), and in laying respectively at and tail gas washing liquid entrance (9), ammonium nitrate slip add in entrance (10) and one section in the downstream canal with slip entrance I (11) entrance.
4. neutralising arrangement as claimed in claim 3, be provided with reaction tubes baffle plate (19) on the inner-wall surface of its described two sections neutralising arrangement reaction tubess (14), and lay respectively in the gas ammonia entrance I (13), one section and in the downstream canal of slip entrance II (15) and gas ammonia entrance II (16) entrance.
5. such as claim 3 or 4 described neutralising arrangements, its described downtake baffle plate (18) is 93 with the angle that axially arranges of reaction tubes baffle plate (19)
0～160
0Between.
6. neutralising arrangement as claimed in claim 1, its described two sections neutralising arrangement slurry outlets (6) are that it is higher than 1 meter that the circulation slip adds mouthful (17), and are positioned under the slip entrance (3).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201220320544 CN202671209U (en) | 2012-07-04 | 2012-07-04 | Mother liquor ammonia neutralization device for nitric phosphate production |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201220320544 CN202671209U (en) | 2012-07-04 | 2012-07-04 | Mother liquor ammonia neutralization device for nitric phosphate production |
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| CN202671209U true CN202671209U (en) | 2013-01-16 |
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| CN 201220320544 Expired - Lifetime CN202671209U (en) | 2012-07-04 | 2012-07-04 | Mother liquor ammonia neutralization device for nitric phosphate production |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102924128A (en) * | 2012-07-04 | 2013-02-13 | 天脊煤化工集团股份有限公司 | Neutralization apparatus for nitric phosphate fertilizer production mother liquid ammonia neutralization process |
| CN109160828A (en) * | 2018-08-22 | 2019-01-08 | 贵州芭田生态工程有限公司 | The neutralization of ammonia twice of mother liquor, method for concentration in Phosphate Fertilizer Nitrate with Frozen Method technical process |
| CN109485461A (en) * | 2018-10-17 | 2019-03-19 | 贵州芭田生态工程有限公司 | Phosphorus ore acid hydrolysis waste gas absorption and utilization method neutralize mother liquor and phosphate fertilizer preparation method |
| CN110589917A (en) * | 2019-09-30 | 2019-12-20 | 广东闻扬环境科技有限公司 | Forced circulation separator |
-
2012
- 2012-07-04 CN CN 201220320544 patent/CN202671209U/en not_active Expired - Lifetime
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102924128A (en) * | 2012-07-04 | 2013-02-13 | 天脊煤化工集团股份有限公司 | Neutralization apparatus for nitric phosphate fertilizer production mother liquid ammonia neutralization process |
| CN102924128B (en) * | 2012-07-04 | 2014-09-10 | 天脊煤化工集团股份有限公司 | Neutralization apparatus for nitric phosphate fertilizer production mother liquid ammonia neutralization process |
| CN109160828A (en) * | 2018-08-22 | 2019-01-08 | 贵州芭田生态工程有限公司 | The neutralization of ammonia twice of mother liquor, method for concentration in Phosphate Fertilizer Nitrate with Frozen Method technical process |
| CN109160828B (en) * | 2018-08-22 | 2021-05-28 | 贵州芭田生态工程有限公司 | Method for twice ammonia neutralization and concentration of mother liquor in process of freezing method nitric phosphate fertilizer technology |
| CN109485461A (en) * | 2018-10-17 | 2019-03-19 | 贵州芭田生态工程有限公司 | Phosphorus ore acid hydrolysis waste gas absorption and utilization method neutralize mother liquor and phosphate fertilizer preparation method |
| CN110589917A (en) * | 2019-09-30 | 2019-12-20 | 广东闻扬环境科技有限公司 | Forced circulation separator |
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|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CX01 | Expiry of patent term | ||
| CX01 | Expiry of patent term |
Granted publication date: 20130116 |