CN105175029A - Method for preparing phosphor (potassium) nitrate fertilizer by wet process phosphate sludge acid - Google Patents
Method for preparing phosphor (potassium) nitrate fertilizer by wet process phosphate sludge acid Download PDFInfo
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- CN105175029A CN105175029A CN201510577840.9A CN201510577840A CN105175029A CN 105175029 A CN105175029 A CN 105175029A CN 201510577840 A CN201510577840 A CN 201510577840A CN 105175029 A CN105175029 A CN 105175029A
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Abstract
The invention discloses a method for preparing phosphor (potassium) nitrate fertilizer by wet process phosphate sludge acid. The phosphor nitrate fertilizer is obtained by adding nitric acid or ammonium nitrate into the wet process phosphate sludge acid according to a certain ratio of P2O5/N, introducing ammonia gas, performing action, granulating and drying; or the potassium nitrate fertilizer is obtained by adding a potassium salt into slurry. According to the method, the wet process phosphate sludge acid is fully and effectively utilized; the product structures of the phosphor nitrate fertilizer and the potassium nitrate fertilizer are widened. The prepared phosphor (potassium) nitrate fertilizer meets the standards of GB/T10510-2007; moreover, the preparation process is simple; the operability is high; the reaction process is environment-friendly; waste which is difficult to treat cannot be produced.
Description
Technical field
The invention belongs to Wet-process Phosphoric Acid Production technical field, relate to the recycling of Method for Sludge of Wet-Process Phosphoric Acid acid, specifically relate to a kind of method utilizing Method for Sludge of Wet-Process Phosphoric Acid acid to prepare nitrophosphate fertilizer or phosphorus-potassium nitrate fertilizer.
Background technology
The source of Method for Sludge of Wet-Process Phosphoric Acid acid mainly comprises: the end acid stayed after the clarification of (1) filter acid; (2) when adopting two-stage concentration flow path, 40%P after the first step is concentrated
2o
5underflow after the phosphoric acid clarification of left and right; (3) underflow after concentrated phosphoric acid sedimentation clarification, this is the main source of Method for Sludge of Wet-Process Phosphoric Acid acid; (4) filter-press residues after the press filtration of concentrated phosphoric acid subsider underflow; (5) press filtration of concentrated phosphoric acid subsider underflow and washing after filter-press residues; (6) remaining slag after phosphoric acid ammonification removal of impurities; (7) phosphoric acid by wet process solvent extraction raffinate etc.
Generally, when market conditions are good, sludge acid can be used for producing the products such as 55-MAP, 57-DAP, TSP.But current Fertilizer Market is low, and production capacity surplus, supply exceed demand, and the Powder MAP that the lower grade utilizing sludge acid to produce, added value is lower, TSP, DAP do not have market, causes phosphoric acid by wet process processing enterprise to have to sludge acid to return phosphoric acid reaction tank.Although sludge acid returns phosphoric acid reaction tank for reaction and provides part crystal seed, P
2o
5be recycled utilization, but soluble salt is finally separated out because of supersaturation in clarifying tank or acid tank, then return, redeposition, so repeatedly, form vicious cycle.Soluble salt in acid is in state of saturation for a long time, has buried hidden danger to line clogging, equipment scaling; Due to the excess of soluble salt, the physical deterioration of slip, slip is clamminess, crystallization becomes elongated, and give filtration, concentrate and cause certain difficulty, throughput declines; Meanwhile, to viscosity, the P of product acid
2o
5concentration, solid content all can cause detrimentally affect.Therefore, Method for Sludge of Wet-Process Phosphoric Acid acid how is effectively utilized just to become current Wet-process Phosphoric Acid Production enterprise technical problem urgently to be resolved hurrily.
At present, cold method is that production nitrophosphate fertilizer uses the most extensively, a kind of largest method of founding the factory, and it is with physics freezing method removing Soluble Ca O, also known as Odda method.Its process is: in the acidolysis groove of stainless steel, use HNO
3the decomposing phosphorite by using nitric acid of>=53%; After acid hydrolysis solution separating acid insolubles, deliver in the multiple stage crystallizer tank of stainless steel, indirectly cool with the refrigerant (20%NH3 water or 35%Ca (NO3) 2 solution) that temperature is-15 DEG C, make acid hydrolysis solution temperature drop to about-5 DEG C; Now CaO is just with Ca (NO
3)
24H
2o form crystallization, then, filter is separated, and with cold nitric acid and cold water washing, wash acid and return in acidolysis groove with wash water, the mother liquor after fractional crystallization mainly consists of H
3pO
4, HNO
3with uncrystallized Ca (NO
3)
2deng.The shortcoming of cold method is: 1. technical process is long, plant investment is high, complicated operation.2. pair raw material phosphorus ore requires high, the P of general requirement phosphorus ore
2o
5>32%.And current high-grade phosphorus ore source has difficulties.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, a kind of method utilizing Method for Sludge of Wet-Process Phosphoric Acid acid to prepare nitrophosphate fertilizer or phosphorus-potassium nitrate fertilizer is provided, improves the utilization ratio of sludge acid, widen the product structure that nitric acid phosphorus (potassium) is fertile.
Object of the present invention is achieved by the following technical programs.
Except as otherwise noted, percentage ratio of the present invention is mass percent.
Utilize Method for Sludge of Wet-Process Phosphoric Acid acid to prepare a method for nitrophosphate fertilizer or phosphorus-potassium nitrate fertilizer, comprise the following steps:
(1) according to P
2o
5nitric acid adds in sludge acid than the mass ratio for 1:0.3 ~ 1 by/N, or according to P
2o
5ammonium nitrate adds in sludge acid than the mass ratio for 1:0.5 ~ 2 by/N, obtains slip A;
(2) in slip A, pass into ammonia, then react at 40 ~ 110 DEG C, to pH=5 ~ 8 of reaction system, obtain slip B;
(3) slip B carries out spray granulating, obtains nitrophosphate fertilizer head product;
(4) nitrophosphate fertilizer head product is dry at 70 DEG C ~ 100 DEG C, namely obtain nitrophosphate fertilizer;
(5) or, in the slip B that step (2) obtains, add 20% ~ 25% sylvite in mass ratio, then repeating step (3) and step (4) namely obtain phosphorus-potassium nitrate fertilizer.
Utilize Method for Sludge of Wet-Process Phosphoric Acid acid to prepare a method for nitrophosphate fertilizer or phosphorus-potassium nitrate fertilizer, comprise the following steps:
(1) ammonia is passed in sludge acid, stirring reaction at 40 ~ 110 DEG C, to pH=5 ~ 8 of reaction system, obtain slip C;
(2) by ammonium nitrate according to P
2o
5/ N mass ratio is that the ratio of 1:0.5 ~ 2 adds in slip C, obtains slip D;
(3) slip D carries out spray granulating, obtains nitrophosphate fertilizer head product;
(4) nitrophosphate fertilizer head product is dry at 70 DEG C ~ 100 DEG C, namely obtain nitrophosphate fertilizer;
(5) or, in the slip D that step (2) obtains, add 20% ~ 25% sylvite in mass ratio, then repeating step (3) and step (4) namely obtain phosphorus-potassium nitrate fertilizer.
Utilize Method for Sludge of Wet-Process Phosphoric Acid acid to prepare a method for nitrophosphate fertilizer or phosphorus-potassium nitrate fertilizer, comprise the following steps:
(1) ammonia is passed in sludge acid, stirring reaction at 40 ~ 110 DEG C, to pH=5 ~ 8 of reaction system, obtain slip E;
(2) first drying is carried out, then according to P to slip E
2o
5/ N mass ratio is that the ratio of 1:1 ~ 2 adds solid ammonium nitrate and is dry mixed, and obtains nitrophosphate fertilizer head product;
(3) nitrophosphate fertilizer head product is again through granulating and drying, namely obtains nitrophosphate fertilizer;
(4) or, in nitrophosphate fertilizer head product, add 20% ~ 25% sylvite according to mass ratio, then obtain phosphorus-potassium nitrate fertilizer through granulating and drying.
As optimization, described sylvite is the one in potassium sulfate or Repone K.
As optimization, the solid content of described sludge acid is 15% ~ 45%, P
2o
5content is 20% ~ 45%
As optimization, the mass concentration of described nitric acid is 53% ~ 98%.
Compared with prior art, the present invention has following beneficial effect:
1, nitric acid phosphorus (potassium) fertilizer that the present invention produces is a kind of high-concentration compound fertilizer containing ammonium nitrogen, nitric nitrogen, available phosphorus etc., and compared with conventional composite fertilizer, fertilizer efficiency is fast, specific absorption is high, also has the feature of anti-soil compaction.Have soluble in water, easily (active absorption) absorbed by crops, do not adsorbed by soil colloid, easily outflow with water, easily denitrification occurs, the features such as the absorption of calcium, magnesium, potassium etc. can be promoted.Nitrate fertilizer can be widely used in the base manure of various crop and topdress, and is applicable to various types of soil.
2, sludge acid solid content 15% ~ 45%, P used in the present invention
2o
5content is 20% ~ 45%, wherein also has the middle and trace element of agronomical value containing S, Ca, Mg, Fe etc., and the high efficiency nutritious element of suitable for plant growth.Nitric acid phosphorus (potassium) fertilizer obtained with it meets GB/T10510-2007 standard, and preparation technology is simple, and workable, reaction process environmental protection, can not produce reluctant waste.
3, present invention achieves the abundant efficiency utilization to Method for Sludge of Wet-Process Phosphoric Acid, widened the product structure of phosphorus-potassium nitrate fertilizer and nitrophosphate fertilizer, while optimization promotes traditional product, separately ward off and utilize new way, reach the object of the updating and upgrading of a product.
Accompanying drawing explanation
Fig. 1 is the process flow diagram of the embodiment of the present invention 1 to 5;
Fig. 2 is the process flow diagram of the embodiment of the present invention 6 to 8;
Fig. 3 is the process flow diagram of the embodiment of the present invention 9 and 10.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in further detail, but drawings and Examples are not limited to the technical solution.
Embodiment 1:
Nitrophosphate fertilizer is prepared in Method for Sludge of Wet-Process Phosphoric Acid acid, comprises following preparation process:
S1: press P in the reactor
2o
5/ N than 1:0.3 add solid content be 15% sludge acid and concentration be the nitric acid of 53%, abundant stirring and dissolving, obtains slip A;
S2: pass into ammonia in the slip A that step S1 obtains, controls temperature of reaction 90 DEG C, to the pH=6 of reaction system, obtains slip B;
S3: the slip B obtained by step S2 carries out spray granulating, obtains nitrophosphate fertilizer head product;
S4: the nitrophosphate fertilizer head product obtained by step S3 carries out drying, namely obtains nitrophosphate fertilizer, its product specification: 23-23-0, total nutrient is 46.
Embodiment 2:
Nitrophosphate fertilizer is prepared in Method for Sludge of Wet-Process Phosphoric Acid acid, comprises following preparation process:
S1: press P in the reactor
2o
5/ N than 1:0.5 add solid content be 30% sludge acid and concentration be the nitric acid of 60%, abundant stirring and dissolving, obtains slip A;
S2: pass into ammonia in the slip A that step S1 obtains, controls temperature of reaction 100 DEG C, to the pH=6 of reaction system, obtains slip B;
S3: the slip B obtained by step S2 carries out spray granulating, obtains nitrophosphate fertilizer head product;
S4: the nitrophosphate fertilizer head product obtained by step S3 carries out drying, namely obtains nitrophosphate fertilizer, its product specification: 20-20-0, total nutrient is 40.
Embodiment 3:
Nitrophosphate fertilizer is prepared in Method for Sludge of Wet-Process Phosphoric Acid acid, comprises following preparation process:
S1: press P in the reactor
2o
5/ N than 1:1 add solid content be 45% sludge acid and concentration be the nitric acid of 68%, abundant stirring and dissolving, obtains slip A;
S2: pass into ammonia in the slip A that step S1 obtains, controls temperature of reaction 110 DEG C, to the pH=7 of reaction system, obtains slip B;
S3: the slip B obtained by step S2 carries out spray granulating, obtains nitrophosphate fertilizer head product;
S4: the nitrophosphate fertilizer head product obtained by step S3 carries out drying, namely obtains nitrophosphate fertilizer, its product specification: 27-13.5-0, total nutrient is 41.
Embodiment 4:
Nitrophosphate fertilizer is prepared in Method for Sludge of Wet-Process Phosphoric Acid acid, comprises following preparation process:
S1: press P in the reactor
2o
5/ N adds than 1:0.7 sludge acid and the ammonium nitrate that solid content is 15%, and abundant stirring and dissolving, obtains slip A;
S2: pass into ammonia in the slip A that step S1 obtains, controls temperature of reaction 40 DEG C, to the pH=6 of reaction system, obtains slip B;
S3: the slip B obtained by step S2 carries out spray granulating, obtains nitrophosphate fertilizer head product;
S4: the nitrophosphate fertilizer head product obtained by step S3 carries out drying, namely obtains nitrophosphate fertilizer, its product specification: 23-23-0, total nutrient is 41.
Embodiment 5:
Phosphorus-potassium nitrate fertilizer is prepared in Method for Sludge of Wet-Process Phosphoric Acid acid, comprises following preparation process:
S1: press P in the reactor
2o
5/ N adds sludge acid and the ammonium nitrate that solid content is 30%, abundant stirring and dissolving than for 1:2, obtains slip A;
S2: pass into ammonia in the slip A that step S1 obtains, controls temperature of reaction 60 DEG C, to the pH=8 of reaction system, obtains slip B;
S3: add 20% potassium sulfate in mass ratio in the slip B obtained by step S2, carry out spray granulating, obtain phosphorus-potassium nitrate fertilizer head product;
S4: the phosphorus-potassium nitrate fertilizer head product obtained by step S3 carries out drying, namely obtains phosphorus-potassium nitrate fertilizer, its product specification: 22-10-10, total nutrient is 42.
Embodiment 6:
Nitrophosphate fertilizer is prepared in Method for Sludge of Wet-Process Phosphoric Acid acid, comprises the following steps:
S1: add the sludge acid that solid content is 15% in the reactor, passes into ammonia and controls temperature of reaction 40 DEG C, to the pH=5 of reaction system, obtain slip C;
S2: press P in slip C
2o
5/ N adds ammonium nitrate solid than 1:0.5, obtains slip D;
S3: the slip D obtained by step S2 carries out spray granulating, obtains nitrophosphate fertilizer head product;
S4: the nitrophosphate fertilizer head product obtained by step S3 carries out drying, namely obtains nitrophosphate fertilizer, its product specification: 23-23-0, total nutrient is 46.
Embodiment 7:
The method of nitrophosphate fertilizer is prepared in Method for Sludge of Wet-Process Phosphoric Acid acid, comprises the following steps:
S1: add the sludge acid that solid content is 30% in the reactor, passes into ammonia and controls temperature of reaction 70 DEG C, to the pH=6 of reaction system, obtain slip C;
S2: press P in slip C
2o
5/ N adds ammonium nitrate solid than 1:0.9, obtains slip D;
S3: the slip D obtained by step S2 carries out spray granulating, obtains nitrophosphate fertilizer head product;
S4: the nitrophosphate fertilizer head product obtained by step S3 carries out drying, namely obtains nitrophosphate fertilizer, its product specification: 20-20-0, total nutrient is 40.
Embodiment 8:
Phosphorus-potassium nitrate fertilizer is prepared in Method for Sludge of Wet-Process Phosphoric Acid acid, comprises the following steps:
S1: add the sludge acid that solid content is 45% in the reactor, passes into ammonia and controls temperature of reaction 100 DEG C, to the pH=7 of reaction system, obtain slip C;
S2: press P in slip C
2o
5/ N adds ammonium nitrate solid than 1:2, obtains slip D;
S3: add 25% Repone K in mass ratio in the slip D obtained by step S2, carry out spray granulating, obtain phosphorus-potassium nitrate fertilizer head product;
S4: the phosphorus-potassium nitrate fertilizer head product obtained by step S3 carries out drying, namely obtains phosphorus-potassium nitrate fertilizer, its product specification: 20-10-10, total nutrient is 40.
Embodiment 9:
Nitrophosphate fertilizer is prepared in Method for Sludge of Wet-Process Phosphoric Acid acid, comprises the following steps:
S1: get solid content 15% sludge acid in the reactor, pass into ammonia control temperature of reaction 60 DEG C, to the pH=5 of reaction system, obtain slip E;
S2: slip E is carried out drying, obtains product F;
S3: according to P
2o
5/ N adds ammonium nitrate solid than 1:1, stirs and obtains nitrophosphate fertilizer product through granulating and drying again, its product specification: 20-20-0, and total nutrient is 40.
Embodiment 10:
Phosphorus-potassium nitrate fertilizer is prepared in Method for Sludge of Wet-Process Phosphoric Acid acid, comprises the following steps:
S1: get solid content 30% sludge acid in the reactor, pass into ammonia control temperature of reaction 100 DEG C, to the pH=6 of reaction system, obtain slip E;
S2: slip E is carried out drying, obtains product F;
S3: according to P
2o
5/ N adds ammonium nitrate solid than 1:2, and adds 20% potassium hydroxide according to mass ratio, and after stirring, granulating and drying obtains phosphorus-potassium nitrate fertilizer product, its product specification: 22-10-10, and total nutrient is 42.
Above-described embodiment is only for example of the present invention is described, and is not limitation of the invention.For those of ordinary skill in the field, other multi-form changes can also be made on the basis of the above description.Here cannot give exhaustive to all embodiments.Every belong to technical scheme of the present invention the apparent change of amplifying out or variation be still in the row of protection scope of the present invention.
Claims (6)
1. utilize Method for Sludge of Wet-Process Phosphoric Acid acid to prepare a method for nitrophosphate fertilizer or phosphorus-potassium nitrate fertilizer, comprise the following steps:
(1) according to P
2o
5nitric acid adds in sludge acid than the mass ratio for 1:0.3 ~ 1 by/N, or according to P
2o
5ammonium nitrate adds in sludge acid than the mass ratio for 1:0.5 ~ 2 by/N, obtains slip A;
(2) in slip A, pass into ammonia, then react at 40 ~ 110 DEG C, to pH=5 ~ 8 of reaction system, obtain slip B;
(3) slip B carries out spray granulating, obtains nitrophosphate fertilizer head product;
(4) nitrophosphate fertilizer head product is dry at 70 DEG C ~ 100 DEG C, namely obtain nitrophosphate fertilizer;
(5) or, in the slip B that step (2) obtains, add 20% ~ 25% sylvite in mass ratio, then repeating step (3) and step (4) namely obtain phosphorus-potassium nitrate fertilizer.
2. the method utilizing Method for Sludge of Wet-Process Phosphoric Acid acid to prepare nitrophosphate fertilizer or phosphorus-potassium nitrate fertilizer according to claim 1, is characterized in that: the mass concentration of the nitric acid described in step (1) is 53% ~ 98%.
3. utilize Method for Sludge of Wet-Process Phosphoric Acid acid to prepare a method for nitrophosphate fertilizer or phosphorus-potassium nitrate fertilizer, comprise the following steps:
(1) ammonia is passed in sludge acid, stirring reaction at 40 ~ 110 DEG C, to pH=5 ~ 8 of reaction system, obtain slip C;
(2) by ammonium nitrate according to P
2o
5/ N mass ratio is that the ratio of 1:0.5 ~ 2 adds in slip C, obtains slip D;
(3) slip D carries out spray granulating, obtains nitrophosphate fertilizer head product;
(4) nitrophosphate fertilizer head product is dry at 70 DEG C ~ 100 DEG C, namely obtain nitrophosphate fertilizer;
(5) or, in the slip D that step (2) obtains, add 20% ~ 25% sylvite in mass ratio, then repeating step (3) and step (4) namely obtain phosphorus-potassium nitrate fertilizer.
4. utilize Method for Sludge of Wet-Process Phosphoric Acid acid to prepare a method for nitrophosphate fertilizer or phosphorus-potassium nitrate fertilizer, comprise the following steps:
(1) ammonia is passed in sludge acid, stirring reaction at 40 ~ 110 DEG C, to pH=5 ~ 8 of reaction system, obtain slip E;
(2) first drying is carried out, then according to P to slip E
2o
5/ N mass ratio is that the ratio of 1:1 ~ 2 adds solid ammonium nitrate and is dry mixed, and obtains nitrophosphate fertilizer head product;
(3) nitrophosphate fertilizer head product is again through granulating and drying, namely obtains nitrophosphate fertilizer;
(4) or, in nitrophosphate fertilizer head product, add 20% ~ 25% sylvite according to mass ratio, then obtain phosphorus-potassium nitrate fertilizer through granulating and drying.
5. the method for nitrophosphate fertilizer or phosphorus-potassium nitrate fertilizer is prepared in the Method for Sludge of Wet-Process Phosphoric Acid acid that utilizes according to claim 1,3 or 4, it is characterized in that: described sylvite is the one in potassium sulfate or Repone K.
6. the method for nitrophosphate fertilizer or phosphorus-potassium nitrate fertilizer is prepared in the Method for Sludge of Wet-Process Phosphoric Acid acid that utilizes according to claim 1,3 or 4, it is characterized in that: the solid content of described sludge acid is 15% ~ 45%, P
2o
5content is 20% ~ 45%.
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Cited By (3)
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CN106278390A (en) * | 2016-07-19 | 2017-01-04 | 中化化肥有限公司成都研发中心 | A kind of phosphoric acid by wet process acid sludge comprehensive reutilization method |
CN108530175A (en) * | 2018-05-28 | 2018-09-14 | 郑州大学 | A kind of granular compound fertilizer and its production method using the production of phosphoric acid slag acid |
CN110483125A (en) * | 2019-08-02 | 2019-11-22 | 史丹利化肥当阳有限公司 | Utilize the method for waste phosphoric acid production S-based compound fertilizer raw material |
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CN104310364A (en) * | 2014-10-11 | 2015-01-28 | 昆明理工大学 | Comprehensive utilization method of phosphoric acid sludge |
CN104649724A (en) * | 2015-01-27 | 2015-05-27 | 瓮福(集团)有限责任公司 | Production method of calcium superphosphate |
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CN103073344A (en) * | 2013-01-23 | 2013-05-01 | 天脊煤化工集团股份有限公司 | Production method for high-concentration defluorinate nitronitrogen phosphorus and potassium compound fertilizer |
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CN106278390A (en) * | 2016-07-19 | 2017-01-04 | 中化化肥有限公司成都研发中心 | A kind of phosphoric acid by wet process acid sludge comprehensive reutilization method |
CN108530175A (en) * | 2018-05-28 | 2018-09-14 | 郑州大学 | A kind of granular compound fertilizer and its production method using the production of phosphoric acid slag acid |
CN110483125A (en) * | 2019-08-02 | 2019-11-22 | 史丹利化肥当阳有限公司 | Utilize the method for waste phosphoric acid production S-based compound fertilizer raw material |
CN110483125B (en) * | 2019-08-02 | 2022-03-04 | 史丹利化肥当阳有限公司 | Method for producing raw material for sulfur-based compound fertilizer by using waste phosphoric acid |
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