CN104355296A - Method for producing high-quality enriched superphosphate as byproduct in production of feed grade calcium hydrophosphate - Google Patents
Method for producing high-quality enriched superphosphate as byproduct in production of feed grade calcium hydrophosphate Download PDFInfo
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- CN104355296A CN104355296A CN201410565026.0A CN201410565026A CN104355296A CN 104355296 A CN104355296 A CN 104355296A CN 201410565026 A CN201410565026 A CN 201410565026A CN 104355296 A CN104355296 A CN 104355296A
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Abstract
The invention relates to a method for producing high-quality enriched superphosphate as a byproduct in the production of feed grade calcium hydrophosphate. The method adopts the following technological processes: 1), using low and middle grade phosphate containing 21-25% of phosphorus pentoxide, ferric oxide, aluminum oxide and magnesium oxide as a raw materials, wherein the content of the ferric oxide, the aluminum oxide and the magnesium oxide is more than 3.5%; preparing high grade phosphate concentrate after flotation, wherein the content of phosphorus pentoxide is 28-33% and the total content of impurities of oxides of iron, magnesium and aluminum is less than 3.5%; using sulfuric acid and the high grade phosphate concentrate with impurities of iron, magnesium and aluminum removed through floatation as raw materials, preparing a wet-process phosphoric acid containing 8-12% of phosphorus pentoxide through a common dihydrate wet phosphoric acid process method, and the like. Through the adoption of the method, the high phosphorus powder as the byproduct can be produced in the process of purification of the wet-process phosphoric acid, further the high-quality enriched superphosphate is prepared, the production cost is greatly reduced, and the economic benefit is improved.
Description
Technical field
The invention relates to and produce high-grade phosphorus concentrate with mid low grade phosphate rock by floatation process, and be raw material at the high phosphoric fertilizer of part produced by high-grade phosphorus heading production calcium hydrophosphate fodder process, the nitration mixture adding a small amount of phosphoric acid and sulfuric acid again produces the method for high-quality double superphosphate, belongs to phosphate fertilizer product manufacturing field.
Background technology
Double superphosphate utilizes sulfuric acid, phosphoric acid or spent acid to be mixed with certain density phosphate rock decomposition by a certain percentage to obtain, and product composition is mainly the hydrate Ca (H of monocalcium phosphate
2pO
4)
2h
2the compositions such as O and a small amount of free phosphoric acid, anhydrous calciumsulphate and tertiary iron phosphate aluminium.
Domestic production double superphosphate, the method all adding concentrated phosphoric acid slag to add sulfuric acid or higher-grade phosphorus ore containing higher-grade phosphorus ore in more than Vanadium Pentoxide in FLAKES 28-31% is produced.Because the method needs more high-grade phosphorus ore, production cost is high, deficiency in economic performance.
It is that twice neutralization is to remove the detrimental impurity such as fluorine, arsenic, lead in phosphoric acid solution with middle higher-grade phosphorus ore and sulfuric acid for waste phosphoric acid by wet process that current internal feed calcium hydrophosphate produces the most general method.Obtain the fertilizer grade secondary calcium phosphate (being commonly called as white fertilizer) containing effective Vanadium Pentoxide in FLAKES 22-25% with rear filtration in first time.Second time neutralization purifies the solid-liquid slip obtained and returns in the phosphoric acid by wet process of first time neutralization.Because the available phosphorus content of fertilizer grade secondary calcium phosphate is low, foreign matter content is high, can only as the raw material of other production composite fertilizers of fertilizer enterprise.Due to fertilizer market collapse, cause the fertilizer grade secondary calcium phosphate of many calcium hydrophosphate fodder enterprises of poor quality, price is low, cannot sell, the a large amount of of fertilizer grade secondary calcium phosphate are caused to overstock, and badly influence the economic benefit of calcium hydrophosphate fodder enterprise, the processed stopping production of most calcium hydrophosphate fodder enterprises or half end-of-life state.
Summary of the invention
The object of the invention is for existing calcium hydrophosphate fodder and double superphosphate production the deficiencies in the prior art part, thering is provided a kind of is that raw material is by producing high-grade phosphorus heading after flotation with mid low grade phosphate rock, again with high-grade phosphorus heading and sulfuric acid for raw material explained hereafter phosphoric acid by wet process routinely, in 3 times, (once neutralization removes a large amount of fluorine with impurity and purification phosphoric acid by wet process, iron, aluminium, the low phosphoric of by-product is fertile simultaneously for arsenic impurities, Two-step neutralization removing small part fluorine, iron, aluminium, arsenic, by-product height phosphoric is fertile simultaneously for the impurity such as magnesium, three neutralizations produce qualified purifying phosphoric acid simultaneously in by-product and slag return first time neutralization and return molten to reclaim phosphorus).The high phosphoric produced with second time neutralization is fertile produces the processing method of high-quality double superphosphate further for raw material.This technological method the high phosphorus powder of a by-product high-quality step of going forward side by side can produce high-quality double superphosphate in wet phosphoric acid purifying process, can significantly reduce production cost, increase economic efficiency.
The present invention is achieved by the following technical solution.
Produce a method for calcium hydrophosphate fodder byproduct in process high-quality double superphosphate, feature of the present invention adopts following technological process:
1) be, raw material with the mid low grade phosphate rock containing Vanadium Pentoxide in FLAKES 21-25% and ferric oxide, aluminum oxide, magnesium oxide total content more than 3.5%, by producing the high-quality phosphorus concentrate of phosphorus pentoxide content 28-33%, iron, aluminium, magnesium oxide total impurities less than 3.5% after flotation;
With the high-quality phosphorus concentrate after flotation removing iron, aluminium, magnesium addition and sulfuric acid for raw material, wet phosphoric acid by dihydrate processing method produces the phosphoric acid by wet process containing Vanadium Pentoxide in FLAKES 8-12% routinely;
2) phosphoric acid by wet process, with back produced for raw material, by three times and purification of wet process phosphoric acid to produce qualified purifying phosphoric acid as the raw material producing calcium hydrophosphate fodder; To carry out in first time and time, with in 10-20% water-ground limestone slip and phosphoric acid by wet process, control pH value 1.5-1.9, control temperature of reaction 30-45 DEG C, reaction times 1.0-3.0 hour;
3), by completely reacted and slurry filtration, will the solids obtained dry after obtain the fertilizer grade phosphoric powder of 20-25%; The filtrate (first purifying phosphoric acid) of remove portion fluorine, iron, aluminium and the impurity such as arsenic, lead makes the raw material of next step purification;
4), with containing in the liming of 2-5% and first time the first purifying phosphoric acid that obtains, control pH value 1.9-2.5, control temperature of reaction 30-45 DEG C, reaction times 1.0-2.0 hour;
5), by completely reacted and slurry filtration, the solids in removing slip, obtains the high phosphoric powder containing effective P33-37% after oven dry; The filtrate removing most of fluorine, iron, aluminium and the impurity such as arsenic, lead is done in next step third time and purification and produce the raw material of calcium hydrophosphate fodder;
6), with second time neutralization purification wait until containing the high phosphoric powder of effective P33-37% for raw material, add the concentrated phosphoric acid of the 10-20% accounting for its quantity of goods produced and the nitration mixture of industrial sulphuric acid, after reaction, slaking, the high phosphoric producing 35-39% is fertile;
7), previous step nitration mixture used refers to the concentrated phosphoric acid of 45% and the industrial sulphuric acid of 98%, adds the industrial sulphuric acid of 5-15% in concentrated phosphoric acid;
8), with the high phosphoric fertilizer of 35-39% for raw material, add the normal superphosphate of part containing available phosphorus 12%, produce the high-quality double superphosphate product containing available phosphorus 25%, 31%, 35% respectively.
This Technology is compared with calcium superphosphate production process method with calcium hydrophosphate fodder common at present, has following beneficial effect:
1. be, raw material with the mid low grade phosphate rock containing Vanadium Pentoxide in FLAKES 21-25% and ferric oxide, aluminum oxide, magnesium oxide total content more than 3.5%, by producing the high-quality phosphorus concentrate of phosphorus pentoxide content 28-33%, iron alumina-magnesia oxide impurity total amount less than 3.5% after flotation.Owing to eliminating the impurity of phosphorus ore in floatation process, ensure that rear operation produce in phosphoric acid by wet process, calcium hydrophosphate fodder quality, in and the high phosphorus powder of scavenging process by-product contain that effect phosphorus is high, reactive behavior good.
2, phosphoric acid by wet process twice defluorinate of routine purification is changed into three defluorinates purification.And the high phosphoric powder that foreign matter content is low, available phosphorus content is high second time produced is as the raw material producing the rich calcium of high-quality.Its feature comprises:
(1) in first time and in purification of wet process phosphoric acid process, first to use in 10-20% water-ground limestone slip and rare phosphoric acid by wet process to pH value 1.5-1.9, the impurity such as most of fluorine, iron, aluminium, arsenic in removing phosphoric acid by wet process, accounts for the 70-30% with slag total amount in traditional hydrogen calcium technique one section with slag in the solid of generation.Common fertilizer calcium hydrophosphate is obtained, as the raw material of composite fertilizer after drying.
(2) second time neutralizes in the liming of purification 2-5% and for the first time and crosses cleaner liquid, and after the Two-step neutralization slag drying obtained, its available phosphorus reaches 33-37%.The amount of Two-step neutralization slag accounts for the 30-70% with slag total amount in traditional hydrogen calcium technique one section.The foreign matter content such as iron, aluminium be significantly less than traditional hydrogen calcium technique produce in and the content of slag.
(3) purify the high phosphoric powder that obtains for raw material with second time neutralization, after adding the concentrated phosphoric acid of 10-20% and the mixing acid of sulfuric acid, the phosphate fertilizer of the high content of phosphorus of 35-39% can be produced.In nitration mixture, add sulfuric acid, the reactive behavior of material can be improved and improve the water-soluble phosphorus of phosphate fertilizer.After adding a certain amount of 12% general calcium again, the rich calcium superphosphate containing available phosphorus 25%, 31%, 35% can be produced respectively.Not only transportation cost is low to produce high-quality double superphosphate, can also solve a difficult problem for home sale, and can export goods and earn foreign currency.Solve the difficult problem being difficult to rich calcium superphosphate processed with mid low grade phosphate rock thus.
3, the technology of the present invention is by improving calcium hydrophosphate fodder some processes condition, produces the fertilizer grade secondary calcium phosphate of high-quality, has both solved the process of common low-quality fertilizer grade secondary calcium phosphate and has sold a difficult problem, and can also produce the double superphosphate of high-quality.
4, the technology of the present invention can realize the object producing high-quality double superphosphate product with mid low grade phosphate rock, and the technology of the present invention can realize the maximization of calcium hydrophosphate fodder economic benefit, is the technology that current calcium hydrophosphate fodder industry has application value most.
Accompanying drawing explanation
Fig. 1 is production technological process of the present invention.
Embodiment
See Fig. 1, a kind of method of producing calcium hydrophosphate fodder byproduct in process high-quality double superphosphate, feature of the present invention adopts following technological process:
1) be, raw material with the mid low grade phosphate rock containing Vanadium Pentoxide in FLAKES 21-25% and ferric oxide, aluminum oxide, magnesium oxide total content more than 3.5%, by producing the high-quality phosphorus concentrate of phosphorus pentoxide content 28-33%, iron alumina-magnesia oxide impurity total amount less than 3.5% after flotation;
With the high-quality phosphorus concentrate after flotation removing iron magnalium impurity and sulfuric acid for raw material, wet phosphoric acid by dihydrate processing method produces the phosphoric acid by wet process containing Vanadium Pentoxide in FLAKES 8-12% routinely;
2) phosphoric acid by wet process, with back produced for raw material, by three times and purification of wet process phosphoric acid to produce qualified purifying phosphoric acid as the raw material producing calcium hydrophosphate fodder; To carry out in first time and time, with in 10-20% water-ground limestone slip and phosphoric acid by wet process, control pH value 1.5-1.9, control temperature of reaction 30-45 DEG C, reaction times 1.0-3.0 hour;
3), by completely reacted and slurry filtration, solids obtains the fertilizer grade phosphoric powder of 20-25% after drying; The filtrate (first purifying phosphoric acid) of remove portion fluorine, iron, aluminium and the impurity such as arsenic, lead makes the raw material of next step purification;
4), with containing in the liming of 2-5% and for the first time with the first purifying phosphoric acid obtained, control pH value 1.9-2.5, control temperature of reaction 30-45 DEG C, reaction times 1.0-2.0 hour;
5), by completely reacted and slurry filtration, the solids in removing slip, obtains the high phosphoric powder containing effective P33-37% after oven dry; The filtrate removing most of fluorine, iron, aluminium and the impurity such as arsenic, lead is done in next step third time and purification and produce the raw material of calcium hydrophosphate fodder;
6), with second time neutralization purification wait until containing the high phosphoric powder of effective P33-37% for raw material, add the concentrated phosphoric acid of the 10-20% accounting for its quantity of goods produced and the nitration mixture of industrial sulphuric acid, after reaction, slaking, the high phosphoric producing 35-39% is fertile;
7), previous step nitration mixture used refers to the concentrated phosphoric acid of 45% and the industrial sulphuric acid of 98%, adds the industrial sulphuric acid of 5-15% in strong phosphoric acid;
8), with the high phosphoric fertilizer of 35-39% for raw material, add the normal superphosphate of part containing available phosphorus 12%, produce the high-quality double superphosphate product containing available phosphorus 25%, 31%, 35% respectively.
Case study on implementation one
1, with the phosphorus ore of grade 23.3% for raw material, select through flotation the phosphoric acid by wet process producing 9.1% after demagging, by the technology of the present invention, to pH value 1.6 in one section of coarse whiting, then carry out one section of secondary limestone vegetation to pH value 2.1, produce the high phosphorus powder containing available phosphorus 34.2%;
2, every 100 parts of high phosphorus powders add 18.6 parts containing the phosphoric acid of Vanadium Pentoxide in FLAKES 42.5% and the nitration mixture (adding the sulfuric acid of 6% in strong phosphoric acid) of sulfuric acid, produce the high phosphate fertilizer containing available phosphorus 35.5%;
3,74.5 parts of general calcium containing available phosphorus 12.3% are added in the high phosphate fertilizer produced at 100 parts of backs, its available phosphorus content 25.6% of the double superphosphate produced, water-soluble phosphorus 16.6%, free acid content 6.5%.Quality product reaches the technical requirements of salable product powdery double superphosphate product.
Case study on implementation two
1, with the phosphorus ore of grade 23.9% for raw material, select through flotation the phosphoric acid by wet process producing 10.2% after demagging, by the technology of the present invention, to pH value 1.7 in first time coarse whiting, then carry out second time limestone vegetation to pH value 2.3, produce the high phosphorus powder containing available phosphorus 35.8%;
2, every 100 parts of high phosphorus powders add 34.1 parts containing the phosphoric acid of Vanadium Pentoxide in FLAKES 41.3% and the nitration mixture (adding the sulfuric acid of 9% in strong phosphoric acid) of sulfuric acid, produce the high phosphate fertilizer containing available phosphorus 37.2%;
3, add in the high phosphate fertilizer produced at 100 parts of backs 30.3 parts containing effective 12.3% general calcium, its available phosphorus content 31.4% of the double superphosphate produced, water-soluble phosphorus 20.4%, free acid content 6.6%.Quality product reaches the technical requirements of acceptable end product powdery double superphosphate product.
Case study on implementation three
1, with the phosphorus ore of grade 24.6% for raw material, select through flotation the phosphoric acid by wet process producing 11.5% after demagging, by the technology of the present invention, to pH value 1.9 in first time coarse whiting, then carry out second time limestone vegetation to pH value 2.4, produce the high phosphorus powder containing available phosphorus 36.7%;
2, every 100 parts of high phosphorus powders add 118.7 parts containing the phosphoric acid of Vanadium Pentoxide in FLAKES 40.2% and the nitration mixture (adding the sulfuric acid of 12% in strong phosphoric acid) of sulfuric acid, produce the high phosphate fertilizer containing available phosphorus 38.6%;
3, add in the high phosphate fertilizer produced at 100 parts of backs 14.2 parts containing effective 12.1% general calcium, its available phosphorus content 35.3% of the double superphosphate produced, water-soluble phosphorus 22.5%, free acid content 6.8%.Quality product reaches the technical requirements of premium grads powdery double superphosphate product.
Claims (1)
1. produce a method for calcium hydrophosphate fodder byproduct in process high-quality double superphosphate, feature of the present invention is, adopts following technological process:
1) be, raw material with the mid low grade phosphate rock containing Vanadium Pentoxide in FLAKES 21-25% and ferric oxide, aluminum oxide, magnesium oxide total content more than 3.5%, by producing the high-quality phosphorus concentrate of phosphorus pentoxide content 28-33%, iron alumina-magnesia oxide impurity total amount less than 3.5% after flotation;
With the high-quality phosphorus concentrate after flotation removing iron magnalium impurity and sulfuric acid for raw material, wet phosphoric acid by dihydrate processing method produces the phosphoric acid by wet process containing Vanadium Pentoxide in FLAKES 8-12% routinely;
2) phosphoric acid by wet process, with back produced for raw material, by three times and purification of wet process phosphoric acid to produce qualified purifying phosphoric acid as the raw material producing calcium hydrophosphate fodder; To carry out in first time and time, with in 10-20% water-ground limestone slip and phosphoric acid by wet process, control pH value 1.5-1.9, control temperature of reaction 30-45 DEG C, reaction times 1.0-3.0 hour;
3), by completely reacted and slurry filtration, will the solids obtained dry after obtain the fertilizer grade phosphoric powder of 20-25%; The filtrate of remove portion fluorine, iron, aluminium and arsenic, plumbous impurity makes the raw material of next step purification;
4), with containing in the liming of 2-5% and for the first time with the first purifying phosphoric acid obtained, control pH value 1.9-2.5, control temperature of reaction 30-45 DEG C, reaction times 1.0-2.0 hour;
5), by completely reacted and slurry filtration, the solids in removing slip, obtains the high phosphoric powder containing effective P33-37% after oven dry; Remove most of fluorine, iron, aluminium and arsenic, the filtrate of plumbous impurity does in next step third time and purification and produce the raw material of calcium hydrophosphate fodder;
6), with second time neutralization purification wait until containing the high phosphoric powder of effective P33-37% for raw material, add the concentrated phosphoric acid of the 10-20% accounting for its quantity of goods produced and the nitration mixture of industrial sulphuric acid, after reaction, slaking, the high phosphoric producing 35-39% is fertile;
7), previous step nitration mixture used refers to the concentrated phosphoric acid of 45% and the industrial sulphuric acid of 98%, adds the industrial sulphuric acid of 5-15% in strong phosphoric acid;
8), with the high phosphoric fertilizer of 35-39% for raw material, add the normal superphosphate of part containing available phosphorus 12%, produce the high-quality double superphosphate product containing available phosphorus 25%, 31%, 35% respectively.
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| CN201410565026.0A CN104355296A (en) | 2014-10-22 | 2014-10-22 | Method for producing high-quality enriched superphosphate as byproduct in production of feed grade calcium hydrophosphate |
| CN201510042909.8A CN104649242B (en) | 2014-10-22 | 2015-01-28 | A kind of method producing calcium hydrophosphate fodder byproduct in process high-quality double superphosphate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106064809A (en) * | 2016-05-27 | 2016-11-02 | 云南派博科技有限公司 | A kind of high-temperature gas directly heats the method that concentrated wet-process phosphoric acid prepares peroxophosphoric acid |
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| CN106006594B (en) * | 2016-05-24 | 2018-06-26 | 湖州展望药业有限公司 | A kind of production method of medicinal calcium phosphate dibasic anhydrous |
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| CN1206702A (en) * | 1998-04-27 | 1999-02-03 | 威远县磷钙饲料厂 | Proparational process for continuous producing calcium hydrogen phosphate |
| CN102020256B (en) * | 2010-11-22 | 2012-05-23 | 马健 | Method for producing industrial and agricultural monoammonium phosphate and magnesium ammonium phosphate with wet-process phosphoric acid |
| CN103880513B (en) * | 2014-04-04 | 2015-11-18 | 中化云龙有限公司 | The method of the water-soluble NPK composite fertilizer of phosphoric acid defluorination coproduction and fodder calcium phosphate salt |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106064809A (en) * | 2016-05-27 | 2016-11-02 | 云南派博科技有限公司 | A kind of high-temperature gas directly heats the method that concentrated wet-process phosphoric acid prepares peroxophosphoric acid |
| CN106064809B (en) * | 2016-05-27 | 2018-10-02 | 云南磷化集团有限公司 | A kind of high-temperature gas directly heats the method that concentrated wet-process phosphoric acid prepares peroxophosphoric acid |
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Application publication date: 20150218 |