CN102659454A - Method for preparing diammonium phosphate and slow release fertilizer by using high-impurity phosphorite - Google Patents
Method for preparing diammonium phosphate and slow release fertilizer by using high-impurity phosphorite Download PDFInfo
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- CN102659454A CN102659454A CN2012101201314A CN201210120131A CN102659454A CN 102659454 A CN102659454 A CN 102659454A CN 2012101201314 A CN2012101201314 A CN 2012101201314A CN 201210120131 A CN201210120131 A CN 201210120131A CN 102659454 A CN102659454 A CN 102659454A
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Abstract
The invention discloses a method for preparing diammonium phosphate and a slow release fertilizer by using high-impurity phosphorite, which is characterized in that the method comprises the following steps: extracting the high-impurity phosphorite by adopting a wet-method phosphate process, directly neutralizing extracted high-impurity phosphate with a basic compound and controlling the neutralization degree of a system to be 0.05-0.7, the temperature to be 60-130 DEG C and the reaction time to be 10-120 minutes; filtering after reaction, producing filter residues into a raw material or a wrapping material of the slow release fertilizer or a blending fertilizer or other slow release fertilizers, concentrating a filtrate and controlling the P2O5 concentration of concentrated solution to be 36-45 percent; and continuously neutralizing the concentrated solution with a basic compound, controlling the neutralization degree of the solution to be 1.3-1.6 and producing neutralized slurry into the diammonium phosphate by adopting a traditional method. The method has the beneficial effects that the prophase flotation process of the high-impurity phosphorite is saved, and the utilization rate of phosphorus resources is improved; the applicability to the phosphorite is strong, and a diammonium phosphate product with excellent quality can be produced as long as the neutralization is properly adjusted.
Description
Technical field
The present invention relates to the method that a kind of high impurity phosphorus ore prepares diammonium phosphate and slow-release fertilizer, belong to the preparation field of ammophos.
Background technology
China's high-quality phosphorus ore proportion is low, is merely 6.4% with data computation in 2005, and high impurity low-grade phosphate ore accounts for 66.2%.Along with the fast development of China's Eleventh Five-Year Plan phosphorous chemical industry industry, the high-quality phosphorus ore remains little at present, and high impurity phosphorus ore can only adopt the method for flotation to improve the quality, otherwise 1,100 ten thousand tons of diammonium phosphate product quality of China can't reach the standard of 18-46-0.The yield of flotation of phosphate rock is generally 80～90%, and the phosphorus loss is serious, and the mine tailing amount is also big, is unfavorable for the comprehensive utilization of resource.Also do not have a kind of otherwise effective technique directly to utilize high impurity phosphorus ore at present, especially utilize high impurity phosphorus ore to produce to satisfy the diammonium phosphate technology of traditional method diammonium phosphate premium grads index among the GB10205-2009.Chinese patent ZL200610021182.6 discloses " adopting acid slime to concentrate the method and the secondary ammoniation reactor of production diammonium phosphate (DAP) ".This patent adopts twice ammonification to produce DAP, and the degree of neutralization of an ammonification is 0.5～1.0, is concentrated to moisture 13～20% to this acid slime; Secondary ammoniation and preparation DAP adopt traditional DAP technology to produce.Its objective is that adopting slip to concentrate practices thrift steam, but deficiency on the implementation is:
1, the phosphoric acid impurity that one time ammonification generated is all in slip, when using raw material for high impurity phosphorus ore, when the slip water cut is 13～30%; Can form thick material; The heat transfer coefficient of concentration heat exchanger sharply descends, and thickening efficiency reduces, and slip can't be carried simultaneously;
When 2, using high impurity phosphorus ore to produce DAP, this technology can't solve the underproof problem of product.For example work as the P in the phosphorus ore
2O
5/ MgO (weight ratio) is lower than at 20 o'clock, and the DAP quality does not reach the index of traditional method diammonium phosphate premium grads among the GB10205-2009.
Application number is that 200810048758.7 patent discloses a kind of " technology of slurry concentrated process coproduction diammonium phosphate and monoammonium phosphate ".This technology and ZL 200610021182.6 be the same also to adopt twice ammonification.One time the ammonification degree of neutralization is 1.0～1.15, and is settlement separate after the ammonification, the thick slurry in bottom with in be used for producing monoammonium phosphate after concentrating with slip; Clear liquid concentrates back secondary ammoniation production diammonium phosphate.This technology has following shortcoming:
1, for high impurity phosphorus ore; The monoammonium phosphate quality that this technology is produced will meet the requirement of slurry concentration process monoammonium phosphate salable product among the GB10205-2009; Must have in a large amount of phosphoric acid and prepare burden, that is to say that the output of monoammonium phosphate will be far longer than diammonium phosphate product with slip; When its major product was monoammonium phosphate, production equipment could normal operation.
2, the same with patent ZL 200610021182.6; After the degree of neutralization of an ammonification reaches 1.0～1.15; The solubleness of phosphorus ammonium in solution sharply descends, and adds that the coproduction diammonium phosphate gets into the thick slurry of high impurity in this slip, makes monoammonium phosphate concentrate and is difficult to carry out;
3, behind the secondary ammoniation (degree of neutralization is 1.4～1.8); Adopt whitewashing drying-granulating machine drying to obtain diammonium phosphate product; This technology has a large amount of ammonia and overflows; Cause the tail gas recycle difficulty, the product of in design library part editor and reuse, being produced simultaneously also is difficult to reach the index of traditional method diammonium phosphate premium grads among the GB10205-2009.
Summary of the invention
The objective of the invention is to the deficiency of prior art and provide a kind of high impurity phosphorus ore to prepare the method for diammonium phosphate and slow-release fertilizer.Be characterized in directly utilizing high impurity phosphorus ore to produce, prepare the diammonium phosphate and the slow-release fertilizer that meet traditional method diammonium phosphate premium grads index among the GB10205-2009.
As everyone knows, traditional method features of DAP production technology is to be concentrated to 46～50% to dilute phosphoric acid (P205 is less than 30%), and with the ammonia neutralization, the control degree of neutralization is about 1.5 then, granulation in ammoniation granulator, and roller drying promptly gets diammonium phosphate product.Along with the dilution of China's phosphorus ore and wherein foreign matter content rising, the diammonium phosphate of being produced traditionally is difficult to National standard.If contain higher magnesium (P in the phosphorus ore
2O
5/ MgO is less than 20) because all being form with carbonate usually, magnesium is present in the phosphorus ore, in the Wet-process Phosphoric Acid Production process, almost all get in the phosphoric acid by wet process, during with such Wet-process Phosphoric Acid Production diammonium phosphate, product does not reach the index of 18-46-0.
The object of the invention by following technical measures realize, wherein said raw material umber except that specified otherwise, be parts by weight.
The method that high impurity phosphorus ore prepares diammonium phosphate and slow-release fertilizer may further comprise the steps:
(1) adopt phosphoric acid by wet process technology to extract high impurity phosphorus ore, the high impurity phosphoric acid that obtains that extracts directly neutralizes with alkaline substance, and the degree of neutralization of the hierarchy of control is 0.05～0.7, in 60～130 ℃ of reactions of temperature, 10～120min;
(2) above-mentioned reactant is filtered, filter cake directly is used as the raw material or the lapping of slow-release fertilizer or production Bulk Blending Fertilizer or other slow-release fertilizer through granulation;
(3) above-mentioned reactant is filtered, filtrating concentrates, the P of control liquid concentrator
2O
5Concentration is 36～45%; Liquid concentrator continues neutralization with alkaline substance, and the degree of neutralization of control solution is 1.3～1.6, and the slip after the neutralization is according to traditional method production diammonium phosphate.
Phosphoric acid by wet process technology is any in two wet technologies, half wet technology, Ban Shui-two wet technology or two water-half wet technology.
Alkaline substance is at least a in liquefied ammonia, gas ammonia, ammoniacal liquor, volatile salt, ammonium hydrogencarbonate, sodium hydroxide, Pottasium Hydroxide, yellow soda ash, salt of wormwood, sodium hydrogencarbonate, saleratus, lime carbonate and the lime.
Filtrating is through further purifying monoammonium phosphate or the diammonium phosphate fertilizer of producing high-grade full water-soluble.
In order to obtain to meet the Secondary ammonium phosphate of GB, according to the difference of foreign matter content in the used phosphorus ore, during the alkaline substance neutralising phosphoric acid, the degree of neutralization of regulation system is to satisfy the requirement of quality product;
Performance test
Adopt GB/T 1871.1-1995 test P
2O
5Content.
Adopt GB/T 1871.2-1995 test Fe
2O
3Content.
Adopt GB/T 1871.3-1995 test Al
2O
3Content.
Adopt the content of GB/T 1871.5-1995 test MgO.
Adopt the content of GB/T 10209-2008 test N.
The present invention has following advantage:
The present invention compared with prior art can directly utilize the production of high impurity low-grade phosphate ore to meet the diammonium phosphate product of GB10205-2009 tradition method diammonium phosphate premium grads index; This technology is not only saved flotation in the early stage operation of high impurity phosphorus ore, improves the utilization ratio of phosphor resource, has also reduced the investment of flotation design library part editor and reuse; Extremely strong to the suitability of phosphorus ore simultaneously, according to the difference of foreign matter content in the used phosphorus ore, as long as suitably adjust degree of neutralization, just can the outstanding DAP product of the quality of production.
Embodiment
Through embodiment the present invention is specifically described below; Be necessary to be pointed out that at this present embodiment only is used for the present invention is further specified; But can not be interpreted as the restriction to protection domain of the present invention, the person skilled in the art in this field can make some nonessential improvement and adjustment according to the content of the invention described above.
Embodiment 1
Take by weighing and contain P
2O
527.3%, R
2O
33.6%, three parts of each 1000g of ground phosphate rock of MgO 2.21% size mixing with 3000g water for first part, and slowly dripping concentration is 93% sulfuric acid 800g, after reaction finishes, filters, and according to three countercurrent washings, the bath water amount is 600ml.Washing water all return extracting system, promptly size mixing with second part of ground phosphate rock, and slowly dripping concentration simultaneously is 93% sulfuric acid 800g, after reaction finishes, filter, and according to three countercurrent washings, the bath water amount is 600ml.Washing water all return extracting system, promptly size mixing with the 3rd part of ground phosphate rock, and slowly dripping concentration simultaneously is 93% sulfuric acid 800g, after reaction finishes, filter, and according to three countercurrent washings, the bath water amount is 600ml.Extract and promptly get impure high phosphoric acid three times.Extraction temperature is controlled at 80 ℃, and each reaction times is 3.0h, promptly according to the technology of two traditional water law phosphoric acid extractions, extracts and contains P
2O
523.0%, MgO1.82%, R
2O
31.56% phosphoric acid solution 3110g.Place the neutralizer of 3500 liters of stainless steel 316L to phosphoric acid, stir down, logical ammonia, the control degree of neutralization is 0.3, reaction times 30min, temperature is controlled at 95 ℃, vacuum filtration, filter cake is a slow-release fertilizer, the filter cake dry weight is: 112.06g contains P
2O
538.3%, N6.2%; Obtain the 2996.6g that filtrates, wherein contain P
2O
522.4%, this filtrating is as the raw material of preparation diammonium phosphate; Concentrate above-mentioned filtrating P in the liquid concentrator
2O
5Be 40%, liquid concentrator places reactor drum, stirs down and with gas ammonia the degree of neutralization of liquid is adjusted to 1.95, after the cooling, uses the absolute ethyl alcohol thorough washing, filter, and vacuum dehydrating at lower temperature, the gained diammonium phosphate product is heavy: 1416.1g wherein contains P
2O
547.4%, N17.1%, the water-soluble rate of phosphorus is 90.6%.
Embodiment 2
Take by weighing and contain P
2O
527.3%, R
2O
33.6%, three parts of each 1000g of ground phosphate rock of MgO 2.21% size mixing with 3000g water for first part, and slowly dripping concentration is 93% sulfuric acid 800g, after reaction finishes, filters, and according to three countercurrent washings, the bath water amount is 600ml.Washing water all return extracting system, promptly size mixing with second part of ground phosphate rock, and slowly dripping concentration simultaneously is 93% sulfuric acid 800g, after reaction finishes, filter, and according to three countercurrent washings, the bath water amount is 600ml.Washing water all return extracting system, promptly size mixing with the 3rd part of ground phosphate rock, and slowly dripping concentration simultaneously is 93% sulfuric acid 800g, after reaction finishes, filter, and according to three countercurrent washings, the bath water amount is 600ml.Extract and promptly get impure high phosphoric acid three times.Extraction temperature is controlled at 85 ℃, and each reaction times is 4.5h, promptly according to the technology of two traditional water law phosphoric acid extractions, extracts and contains P
2O
523.6%, MgO1.91%, R
2O
31.66% phosphoric acid solution 3227g.Place the neutralizer of 3500 liters of stainless steel 316L to phosphoric acid, stir down, add volatile salt, the control degree of neutralization is 0.7, reaction times 10min, and temperature is controlled at 100 ℃, vacuum filtration, filter cake is a slow-release fertilizer, the filter cake dry weight is: 151.9g contains P
2O
540.1%, N8.9%; Obtain the 3072.1g that filtrates, wherein contain P
2O
522.81%, this filtrating is as the raw material of preparation diammonium phosphate; Concentrate above-mentioned filtrating P in the liquid concentrator
2O
5Be 40%, liquid concentrator places reactor drum, stirs down and with gas ammonia the degree of neutralization of liquid is adjusted to 1.95, after the cooling, uses the absolute ethyl alcohol thorough washing, filter, and vacuum dehydrating at lower temperature, the quality of gained diammonium phosphate product reaches the GB requirement.Experimental data and quality product are seen table 1.
Embodiment 3
Take by weighing and contain P
2O
527.3%, R
2O
33.6%, three parts of each 1000g of ground phosphate rock of MgO 2.21% size mixing with 3000g water for first part, and slowly dripping concentration is 93% sulfuric acid 800g, after reaction finishes, filters, and according to three countercurrent washings, the bath water amount is 600ml.Washing water all return extracting system, promptly size mixing with second part of ground phosphate rock, and slowly dripping concentration simultaneously is 93% sulfuric acid 800g, after reaction finishes, filter, and according to three countercurrent washings, the bath water amount is 600ml.Washing water all return extracting system, promptly size mixing with the 3rd part of ground phosphate rock, and slowly dripping concentration simultaneously is 93% sulfuric acid 800g, after reaction finishes, filter, and according to three countercurrent washings, the bath water amount is 600ml.Extract and promptly get impure high phosphoric acid three times.Extraction temperature is controlled at 82 ℃, and each reaction times is 4.0h, promptly according to the technology of two traditional water law phosphoric acid extractions, extracts and contains P
2O
522.3%, MgO 1.62%, R
2O
31.61% phosphoric acid solution 3265g.Place the neutralizer of 3500 liters of stainless steel 316L to phosphoric acid, stir down, ventilation ammonia, the control degree of neutralization is 0.5, reaction times 60min, temperature is controlled at 90 ℃, vacuum filtration, filter cake is a slow-release fertilizer, the filter cake dry weight is: 129.7g contains P
2O
539.3%, N8.1%; Obtain the 3130.0g that filtrates, wherein contain P
2O
521.63%, this filtrating is as the raw material of preparation diammonium phosphate; Concentrate above-mentioned filtrating P in the liquid concentrator
2O
5Be 40%, liquid concentrator places reactor drum, stirs down and with gas ammonia the degree of neutralization of liquid is adjusted to 1.95, after the cooling, uses the absolute ethyl alcohol thorough washing, filter, and vacuum dehydrating at lower temperature, the quality of gained diammonium phosphate product reaches the GB requirement.Experimental data and quality product are seen table 2.
Embodiment 4
Adopt half water law phosphoric acid by wet process technology to extract high impurity phosphorus ore, directly with the lime neutralization, the degree of neutralization of the hierarchy of control is 0.05 to the high impurity phosphoric acid that is extracted, and temperature is 60 ℃, reaction times 120min; The reaction after-filtration, filter residue is used for producing slow-release fertilizer or Bulk Blending Fertilizer, and filtrating concentrates, the P of control liquid concentrator
2O
5Concentration is 36～45%; Adopt liquefied ammonia to continue neutralization, the degree of neutralization of control solution is 1.3, and the slip after the neutralization is according to traditional method diammonium phosphate explained hereafter Secondary ammonium phosphate, and the quality of product reaches the GB requirement.
Embodiment 5
Adopt half water-wet phosphoric acid by dihydrate technology to extract high impurity phosphorus ore, the high impurity phosphoric acid that is extracted need not concentrate directly and neutralize with Pottasium Hydroxide, and the degree of neutralization of the hierarchy of control is 0.7, and temperature is 130 ℃, 10 minutes reaction times; The reaction after-filtration, filter residue is used for producing slow-release fertilizer or Bulk Blending Fertilizer, and filtrating concentrates, the P of control liquid concentrator
2O
5Concentration is 45%; Liquid concentrator adopts ammoniacal liquor to continue neutralization, and the degree of neutralization of control solution is 1.6, and the slip after the neutralization is according to traditional method diammonium phosphate explained hereafter Secondary ammonium phosphate, and the quality of product reaches the GB requirement.
Embodiment 6
Adopt two water-half water law phosphoric acid by wet process technology to extract high impurity phosphorus ore, the high impurity phosphoric acid that is extracted need not concentrate directly and neutralize with yellow soda ash, and the degree of neutralization of the hierarchy of control is 0.35, and temperature is 90 ℃, 70 minutes reaction times; The reaction after-filtration, filter residue is used for producing slow-release fertilizer or Bulk Blending Fertilizer, and filtrating concentrates, the P of control liquid concentrator
2O
5Concentration is 40%; Liquid concentrator adopts gas ammonia to continue neutralization, and the degree of neutralization of control solution is 1.4, and the slip after the neutralization is according to traditional method diammonium phosphate explained hereafter Secondary ammonium phosphate, and the quality of product reaches the GB requirement.
Embodiment 7
Adopt wet phosphoric acid by dihydrate technology to extract high impurity phosphorus ore, the high impurity phosphoric acid that is extracted need not concentrate directly and neutralize with lime carbonate, and the degree of neutralization of the hierarchy of control is 0.15, and temperature is 90 ℃, 80 minutes reaction times; The reaction after-filtration, filter residue is used for producing slow-release fertilizer or Bulk Blending Fertilizer, and filtrating concentrates, the P of control liquid concentrator
2O
5Concentration 36%; Liquid concentrator adopts gas ammonia to continue neutralization, and the degree of neutralization of control solution is 1.4, and the slip after the neutralization is according to traditional method diammonium phosphate explained hereafter Secondary ammonium phosphate, and the quality of product reaches the GB requirement.
Embodiment 8
Adopt wet phosphoric acid by dihydrate technology to extract high impurity phosphorus ore, the high impurity phosphoric acid that is extracted need not concentrate directly and neutralize with saleratus, and the degree of neutralization of the hierarchy of control is 0.15, and temperature is 90 ℃, 80 minutes reaction times; The reaction after-filtration, filter residue is used for producing slow-release fertilizer or Bulk Blending Fertilizer, and filtrating concentrates, the P of control liquid concentrator
2O
5Concentration is 40%; Liquid concentrator adopts gas ammonia to continue neutralization, and the degree of neutralization of control solution is 1.4, and the slip after the neutralization is according to traditional method diammonium phosphate explained hereafter Secondary ammonium phosphate, and the quality of product reaches the GB requirement.
Table 1
Table 2
Claims (4)
1. one kind high impurity phosphorus ore prepares the method for diammonium phosphate and slow-release fertilizer, it is characterized in that this method may further comprise the steps:
(1) adopt phosphoric acid by wet process technology to extract high impurity phosphorus ore, the high impurity phosphoric acid that obtains that extracts directly neutralizes with alkaline substance, and the degree of neutralization of the hierarchy of control is 0.05～0.7, in 60～130 ℃ of reactions of temperature, 10～120min;
(2) above-mentioned reactant is filtered, filter cake directly is used as the raw material or the lapping of slow-release fertilizer or production Bulk Blending Fertilizer or other slow-release fertilizer through granulation;
(3) above-mentioned reactant is filtered, filtrating concentrates, the P of control liquid concentrator
2O
5Concentration is 36～45%; Liquid concentrator continues neutralization with alkaline substance, and the degree of neutralization of control solution is 1.3～1.6, and the slip after the neutralization is according to traditional method production diammonium phosphate.
2. high according to claim 1 impurity phosphorus ore prepares the method for diammonium phosphate and slow-release fertilizer, it is characterized in that phosphoric acid by wet process technology is any in two wet technologies, half wet technology, Ban Shui-two wet technology or two water-half wet technology.
3. the method for high according to claim 1 impurity phosphorus ore production diammonium phosphate and slow-release fertilizer is characterized in that alkaline substance is at least a in liquefied ammonia, gas ammonia, ammoniacal liquor, volatile salt, ammonium hydrogencarbonate, sodium hydroxide, Pottasium Hydroxide, yellow soda ash, salt of wormwood, sodium hydrogencarbonate, saleratus, lime carbonate and the lime.
4. the method for high according to claim 1 impurity phosphorus ore production diammonium phosphate and slow-release fertilizer is characterized in that filtrating through further purifying monoammonium phosphate or the diammonium phosphate fertilizer of producing high-grade full water-soluble.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103435376A (en) * | 2013-07-29 | 2013-12-11 | 山东明瑞化工集团有限公司 | Method and apparatus used for preparing ammonium phosphate fertilizer from phosphoric acid sediment |
| CN104261371A (en) * | 2014-09-01 | 2015-01-07 | 云南云天化国际化工有限公司 | Method for producing diammonium phosphate from high-impurity phosphorite |
| CN105036816A (en) * | 2015-07-28 | 2015-11-11 | 中化化肥有限公司成都研发中心 | Method for adjusting enriched nutrients in monoammonium phosphate through utilizing phosphate flotation tailings |
| CN106904586A (en) * | 2017-01-19 | 2017-06-30 | 赵常然 | A kind of active charcoal bag membrane material and the ammonium of crystal phosphoric acid one, the co-production of two ammoniums |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103435376A (en) * | 2013-07-29 | 2013-12-11 | 山东明瑞化工集团有限公司 | Method and apparatus used for preparing ammonium phosphate fertilizer from phosphoric acid sediment |
| CN104261371A (en) * | 2014-09-01 | 2015-01-07 | 云南云天化国际化工有限公司 | Method for producing diammonium phosphate from high-impurity phosphorite |
| CN104261371B (en) * | 2014-09-01 | 2016-04-20 | 云南云天化国际化工有限公司 | A kind of method by high impurity phosphorus ore production diammonium phosphate |
| CN105036816A (en) * | 2015-07-28 | 2015-11-11 | 中化化肥有限公司成都研发中心 | Method for adjusting enriched nutrients in monoammonium phosphate through utilizing phosphate flotation tailings |
| CN106904586A (en) * | 2017-01-19 | 2017-06-30 | 赵常然 | A kind of active charcoal bag membrane material and the ammonium of crystal phosphoric acid one, the co-production of two ammoniums |
| CN106904586B (en) * | 2017-01-19 | 2019-02-19 | 赵常然 | A kind of co-production of active charcoal bag membrane material and crystal phosphoric acid monoammonium, diammonium |
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