CN104402534A - Method adopting grading equipment to carry out grading treatment on reaction slurry - Google Patents
Method adopting grading equipment to carry out grading treatment on reaction slurry Download PDFInfo
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- CN104402534A CN104402534A CN201410627414.7A CN201410627414A CN104402534A CN 104402534 A CN104402534 A CN 104402534A CN 201410627414 A CN201410627414 A CN 201410627414A CN 104402534 A CN104402534 A CN 104402534A
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- calcium sulfate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/46—Sulfates
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B11/00—Fertilisers produced by wet-treating or leaching raw materials either with acids in such amounts and concentrations as to yield solutions followed by neutralisation, or with alkaline lyes
- C05B11/04—Fertilisers produced by wet-treating or leaching raw materials either with acids in such amounts and concentrations as to yield solutions followed by neutralisation, or with alkaline lyes using mineral acid
- C05B11/06—Fertilisers produced by wet-treating or leaching raw materials either with acids in such amounts and concentrations as to yield solutions followed by neutralisation, or with alkaline lyes using mineral acid using nitric acid (nitrophosphates)
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- Inorganic Chemistry (AREA)
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Abstract
The invention discloses a method adopting grading equipment to carry out a grading treatment on reaction slurry. The calcium sulfate crystal particles are graded according to the particle size. The calcium sulfate with a particle size more than 40 [mu]m is large particle reaction slurry, and the calcium sulfate with a particle size less than 10 [mu]m is small particle reaction slurry. Then a filter aid is added, wherein the filter aid is one or more of perlite, diatomite, humic acid, bentonite, and wood chip. The provided method has prominent economic and social profits.
Description
Technical field
The present invention relates to a kind of stage equipment that adopts and the method for stage treatment is carried out to reaction slurry.
Background technology
Reality is that the grade of phosphorus ore and quality are declining year by year, and enterprise must be faced with use mid low grade phosphate rock.If produced with mid low grade phosphate rock tissue, so existing apparatus, existing technique cannot meet the nitrophosphate fertilizer target level of product quality of production total nutrient >=38%, water-soluble rate >=55%.Therefore, Technology existing apparatus basis developing mid low grade phosphate rock stone production high concentration nitric-phosphate fertilizer has strategic importance.
Cold method calcium depleted product nitrocalcite need be converted into calcium carbonate, and due to wherein containing acid non-soluble substance and organic seston, calcium carbonate can only be stacked or as cement raw material.Chemical precipitation method calcium depleted product is calcium sulfate, and owing to wherein containing acid non-soluble substance and organic seston, calcium sulfate can only be stacked as phosphogypsum.According to existing mining level and consumption estimation, result of study shows: world phosphate can meet the demand in 100 years, but the abundant ore source of Chinese P2O5 >=30% only can use (Zhang Weifeng in 2014, Marvin's is strange, Zhang Fusuo etc., natural resources journal, 2005,20 (3): 378-386; Lu Rukun, soil, 2004,36 (1): 1-4).Along with the continuous minimizing of high-quality phosphorus ore reserves, no matter be domestic or external, phosphorus compound fertilizer enterprise all will be faced with the predicament using low-grade phosphate ore to produce, and is particularly engaged in the enterprise that high concentration nitric-phosphate fertilizer is produced.So, on existing apparatus basis, by development of new operational path, must could solve the technical barrier that low-grade phosphate ore produces qualified nitrophosphate fertilizer, also could adapt to the market structure of China's phosphate rock resource.
Nitrophosphate fertilizer is a kind of nitro phosphor complex, with phosphorus ore, nitric acid and ammonia for raw material generally adopts Phosphate Fertilizer Nitrate with Frozen Method production technique to produce.It is day ridge board Phosphate Fertilizer Production devices that the unique a set of employing cold method production technique of China produces 900000 tons of nitro phosphor complexs per year, and operational path is advanced, and fertilizer variety is good, and agricultural effect is obvious, plays an important role in national economy.From current fertilizer selling price situation, the price of nitrophosphate fertilizer unit nutrient is minimum in various composite fertilizer, has very strong competitive edge.
" a kind of processing method of producing high concentration nitric-phosphate fertilizer " (application number: 200910009223.3), the settlement treatment of acid non-soluble substance has been carried out to acid hydrolysis solution, but wherein still have tiny acid non-soluble substance and organic seston, still substantial help be there is no to the comprehensive utilization of calcium depleted product.The technical process of Phosphate Fertilizer Nitrate with Frozen Method is that phosphorus ore adds that nitric acid carries out acid non-soluble substance precipitate and separate in acidolysis, acid hydrolysis solution, nitrocalcite freezing and crystallizing from acid hydrolysis solution is separated out, nitrocalcite filters, the mother liquor that filters to isolate from nitrocalcite carries out ammonia neutralization, and slip evaporation, then granulation, be drying to obtain nitrophosphate fertilizer product.Nitrophosphate fertilizer product total nutrient is greater than 38%, wherein containing P2O5 ~ 12.5%, and N ~ 25%, other nutrient ~ 2%.This technique is original design requires that raw material phosphorus ore grade is higher, and phosphorus ore quality index must meet P2O5 >=31%, MgO≤1.0%, AI≤10%; The cement mill of digestion waste material calcium carbonate is equipped with.
But along with the minimizing year by year of China's higher-grade phosphate rock resource, the grade of phosphorus ore and quality are declining year by year, China's phosphate rock resource is being classified as later narrow resources in 2010 by country, and China's phosphorus ore 80% is sedimentogeneous rock, and 70% is the collophanite of middle-low grade.
Summary of the invention
In order to solve the problems of the technologies described above, the present invention is achieved through the following technical solutions:
A kind of stage equipment that adopts carries out the method for stage treatment to reaction slurry, stage treatment is carried out to the size of crystal of calcium sulfate particle, the calcium sulfate being greater than 40 μm with particle diameter is macrobead reaction slurry, and the calcium sulfate being less than 10 μm with particle diameter is small-particle reaction slurry; Then add flocculating aids, flocculating aids is one or more in perlite, diatomite, humic acids, wilkinite, wood chip.By mass percentage, the reaction slurry with small-particle calcium sulfate accounts for total slip ratio 80-90% and returns mother liquor degree of depth deliming process, and for crystal of calcium sulfate provides, crystal seed is also grown up further, growing up enters classification cycle next time; Reaction slurry with macrobead calcium sulfate accounts for total slip ratio 70-80% and delivers to calcium sulfate filtration.
Aforesaidly help worry purifying method, preferred scheme is, described flocculating aids is one or more in perlite, diatomite, humic acids, wilkinite, wood chip etc.
Aforesaidly help worry purifying method, preferred scheme is, described flocculating aids add-on is the 0.5-2% of acid hydrolysis solution quality.Preferred 1-1.5%.Be more preferably 1.3%.
The present invention has following characteristics and beneficial effect: the major advantage of this production high concentration nitric-phosphate fertilizer processing method is:
1) increase the method for mother liquor degree of depth deliming operation simple, relatively independent, have a style of one's own, facility investment is low.Be easy to actualizing technology transformation on former Phosphate Fertilizer Nitrate with Frozen Method device;
2) the present invention makes solution liquid liquid filtration velocity increase substantially, and is 10-20 times of the acid hydrolysis solution filtration velocity not adding flocculating aids.The present invention is first filter acid insolubles and organic seston before the acid hydrolysis solution decalcification of decomposing phosphorite by using nitric acid, the pure calcium carbonate of decalcification byproduct terra alba (gypsum) or conversion of calcium nitrate is greatly improved, can sell as filler, high-purity raw product, without phosphogypsum or the discharge of calcium carbonate slag, realize the comprehensive utilization of resource; In acid hydrolysis solution of the present invention, acid non-soluble substance and organic seston are separated thoroughly, and suspended substance decreasing ratio is high, and after arriving more than 99% purification, acid hydrolysis solution suspension content is at below 100mg/L;
3) nitrophosphate fertilizer of available mid low grade phosphate rock production high density; According to calcium sulfate substance crystallization property, deliming process adopts Crystallization Separation equipment, can significantly improve the Particle size and distribution entering filtration procedure calcium sulfate, for the fast filtering of slurry provides favourable condition, thus strainability, scourability have also been obtained raising;
Utilizing mid low grade phosphate rock to produce highly water-soluble compound nitrogen phosphate fertilizer is the inexorable trend that China develops nitrophosphate fertilizer, through the effort of nearly 30 years, China has grasped completely and has digested the production technique of Phosphate Fertilizer Nitrate with Frozen Method, and the ripe of development low-grade phosphate ore production high-quality compound nitrogen phosphate fertilizer, the enforcement of this production high concentration nitric-phosphate fertilizer processing method can be the long term growth of nitrophosphate fertilizer industry and establishes good plinth.
Embodiment
Embodiment 1
Adopt stage equipment to carry out a method for stage treatment to reaction slurry, carry out stage treatment to the size of crystal of calcium sulfate particle, the calcium sulfate with particle diameter 80 μm is macrobead reaction slurry, and the calcium sulfate with particle diameter 1 μm is small-particle reaction slurry; Then add flocculating aids, flocculating aids is one or more in perlite, diatomite, humic acids, wilkinite, wood chip.By mass percentage, the reaction slurry with small-particle calcium sulfate accounts for total slip ratio 80% and returns mother liquor degree of depth deliming process, and for crystal of calcium sulfate provides, crystal seed is also grown up further, growing up enters classification cycle next time; Reaction slurry with macrobead calcium sulfate accounts for total slip ratio 80% and delivers to calcium sulfate filtration.
Embodiment 2
Adopt stage equipment to carry out a method for stage treatment to reaction slurry, carry out stage treatment to the size of crystal of calcium sulfate particle, the calcium sulfate with particle diameter 70 μm is macrobead reaction slurry, and the calcium sulfate with particle diameter 1 μm is small-particle reaction slurry; Then add flocculating aids, flocculating aids is one or more in perlite, diatomite, humic acids, wilkinite, wood chip.By mass percentage, the reaction slurry with small-particle calcium sulfate accounts for total slip ratio 90% and returns mother liquor degree of depth deliming process, and for crystal of calcium sulfate provides, crystal seed is also grown up further, growing up enters classification cycle next time; Reaction slurry with macrobead calcium sulfate accounts for total slip ratio 80% and delivers to calcium sulfate filtration.
Embodiment 3
Adopt stage equipment to carry out a method for stage treatment to reaction slurry, carry out stage treatment to the size of crystal of calcium sulfate particle, the calcium sulfate with particle diameter 80 μm is macrobead reaction slurry, and the calcium sulfate with particle diameter 4 μm is small-particle reaction slurry; Then add flocculating aids, flocculating aids is humic acids.By mass percentage, the reaction slurry with small-particle calcium sulfate accounts for total slip ratio 80% and returns mother liquor degree of depth deliming process, and for crystal of calcium sulfate provides, crystal seed is also grown up further, growing up enters classification cycle next time; Reaction slurry with macrobead calcium sulfate accounts for total slip ratio 70% and delivers to calcium sulfate filtration.
Embodiment 4
Adopt stage equipment to carry out a method for stage treatment to reaction slurry, carry out stage treatment to the size of crystal of calcium sulfate particle, the calcium sulfate with particle diameter 90 μm is macrobead reaction slurry, and the calcium sulfate with particle diameter 2 μm is small-particle reaction slurry; Then add flocculating aids, flocculating aids is wilkinite, wood chip.By mass percentage, the reaction slurry with small-particle calcium sulfate accounts for total slip ratio 90% and returns mother liquor degree of depth deliming process, and for crystal of calcium sulfate provides, crystal seed is also grown up further, growing up enters classification cycle next time; Reaction slurry with macrobead calcium sulfate accounts for total slip ratio 74% and delivers to calcium sulfate filtration.
Embodiment 5
Adopt stage equipment to carry out a method for stage treatment to reaction slurry, carry out stage treatment to the size of crystal of calcium sulfate particle, the calcium sulfate with particle diameter 50 μm is macrobead reaction slurry, and the calcium sulfate with particle diameter 2 μm is small-particle reaction slurry; Then add flocculating aids, flocculating aids is perlite.By mass percentage, the reaction slurry with small-particle calcium sulfate accounts for total slip ratio 82% and returns mother liquor degree of depth deliming process, and for crystal of calcium sulfate provides, crystal seed is also grown up further, growing up enters classification cycle next time; Reaction slurry with macrobead calcium sulfate accounts for total slip ratio 79% and delivers to calcium sulfate filtration.
Embodiment 6
Adopt stage equipment to carry out a method for stage treatment to reaction slurry, carry out stage treatment to the size of crystal of calcium sulfate particle, the calcium sulfate with particle diameter 60 μm is macrobead reaction slurry, and the calcium sulfate with particle diameter 4 μm is small-particle reaction slurry; Then add flocculating aids, flocculating aids is perlite.By mass percentage, the reaction slurry with small-particle calcium sulfate accounts for total slip ratio 90% and returns mother liquor degree of depth deliming process, and for crystal of calcium sulfate provides, crystal seed is also grown up further, growing up enters classification cycle next time; Reaction slurry with macrobead calcium sulfate accounts for total slip ratio 80% and delivers to calcium sulfate filtration.
Embodiment 7
Adopt stage equipment to carry out a method for stage treatment to reaction slurry, carry out stage treatment to the size of crystal of calcium sulfate particle, the calcium sulfate with particle diameter 50 μm is macrobead reaction slurry, and the calcium sulfate with particle diameter 8 μm is small-particle reaction slurry; Then add flocculating aids, flocculating aids is wood chip.By mass percentage, the reaction slurry with small-particle calcium sulfate accounts for total slip ratio 90% and returns mother liquor degree of depth deliming process, and for crystal of calcium sulfate provides, crystal seed is also grown up further, growing up enters classification cycle next time; Reaction slurry with macrobead calcium sulfate accounts for total slip ratio 80% and delivers to calcium sulfate filtration.
Claims (1)
1. one kind adopts stage equipment to carry out the method for stage treatment to reaction slurry, stage treatment is carried out to the size of crystal of calcium sulfate particle, the calcium sulfate being greater than 40 μm with particle diameter is macrobead reaction slurry, and the calcium sulfate being less than 10 μm with particle diameter is small-particle reaction slurry; Then add flocculating aids, flocculating aids is one or more in perlite, diatomite, humic acids, wilkinite, wood chip.By mass percentage, the reaction slurry with small-particle calcium sulfate accounts for total slip ratio 80-90% and returns mother liquor degree of depth deliming process, and for crystal of calcium sulfate provides, crystal seed is also grown up further, growing up enters classification cycle next time; Reaction slurry with macrobead calcium sulfate accounts for total slip ratio 70-80% and delivers to calcium sulfate filtration.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410627414.7A CN104402534A (en) | 2014-11-10 | 2014-11-10 | Method adopting grading equipment to carry out grading treatment on reaction slurry |
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| CN201410627414.7A CN104402534A (en) | 2014-11-10 | 2014-11-10 | Method adopting grading equipment to carry out grading treatment on reaction slurry |
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| CN104402534A true CN104402534A (en) | 2015-03-11 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112704956A (en) * | 2020-12-30 | 2021-04-27 | 金正大生态工程集团股份有限公司 | Method for strengthening separation of acid-insoluble substances in phosphorite decomposed by nitric acid and application of acid-insoluble substances |
Citations (6)
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|---|---|---|---|---|
| SU887555A1 (en) * | 1980-04-11 | 1981-12-07 | Предприятие П/Я Р-6295 | Method of producing complex fertilizer |
| CN101486595A (en) * | 2009-02-25 | 2009-07-22 | 天脊煤化工集团股份有限公司 | Technological process for producing high concentration nitric-phosphate fertilizer |
| CN102133495A (en) * | 2011-01-20 | 2011-07-27 | 山东金正大生态工程股份有限公司 | Method for purifying acidolysis solution by filter aid and polyacrylamide |
| CN102166452A (en) * | 2011-01-20 | 2011-08-31 | 山东金正大生态工程股份有限公司 | Method for filtration-assisted purification of acidolysis solution obtained in the process of decomposing phosphorite by using nitric acid |
| CN103288495A (en) * | 2013-05-16 | 2013-09-11 | 陈和平 | Method for carrying out stage treatment on reaction slurry |
| RU2505478C1 (en) * | 2012-08-31 | 2014-01-27 | Открытое акционерное общество "Научно-исследовательский институт по удобрениям и инсектофунгицидам имени профессора Я.В.Самойлова" (ОАО "НИУИФ") | Method of obtaining extraction phosphoric acid |
-
2014
- 2014-11-10 CN CN201410627414.7A patent/CN104402534A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU887555A1 (en) * | 1980-04-11 | 1981-12-07 | Предприятие П/Я Р-6295 | Method of producing complex fertilizer |
| CN101486595A (en) * | 2009-02-25 | 2009-07-22 | 天脊煤化工集团股份有限公司 | Technological process for producing high concentration nitric-phosphate fertilizer |
| CN102133495A (en) * | 2011-01-20 | 2011-07-27 | 山东金正大生态工程股份有限公司 | Method for purifying acidolysis solution by filter aid and polyacrylamide |
| CN102166452A (en) * | 2011-01-20 | 2011-08-31 | 山东金正大生态工程股份有限公司 | Method for filtration-assisted purification of acidolysis solution obtained in the process of decomposing phosphorite by using nitric acid |
| RU2505478C1 (en) * | 2012-08-31 | 2014-01-27 | Открытое акционерное общество "Научно-исследовательский институт по удобрениям и инсектофунгицидам имени профессора Я.В.Самойлова" (ОАО "НИУИФ") | Method of obtaining extraction phosphoric acid |
| CN103288495A (en) * | 2013-05-16 | 2013-09-11 | 陈和平 | Method for carrying out stage treatment on reaction slurry |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112704956A (en) * | 2020-12-30 | 2021-04-27 | 金正大生态工程集团股份有限公司 | Method for strengthening separation of acid-insoluble substances in phosphorite decomposed by nitric acid and application of acid-insoluble substances |
| CN112704956B (en) * | 2020-12-30 | 2022-11-18 | 金正大生态工程集团股份有限公司 | Method for strengthening separation of acid-insoluble substances in phosphorite decomposed by nitric acid and application of acid-insoluble substances |
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Application publication date: 20150311 |