CN102161602A - Method for preparing phosphorus-magnesium compound fertilizer by utilizing raffinate and phosphate tailings with high magnesium content - Google Patents
Method for preparing phosphorus-magnesium compound fertilizer by utilizing raffinate and phosphate tailings with high magnesium content Download PDFInfo
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- CN102161602A CN102161602A CN201010608653XA CN201010608653A CN102161602A CN 102161602 A CN102161602 A CN 102161602A CN 201010608653X A CN201010608653X A CN 201010608653XA CN 201010608653 A CN201010608653 A CN 201010608653A CN 102161602 A CN102161602 A CN 102161602A
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- compound fertilizer
- magnesium compound
- phosphorus
- raffinate
- fertilizer material
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Abstract
The invention discloses a method for preparing a phosphorus-magnesium compound fertilizer by utilizing raffinate and phosphate tailings with high magnesium content. The method comprises the following steps of: drying and crushing 1,001 to 1,003 parts of phosphate tailings with high magnesium content which contains 4 to 7 mass percent of P2O5 and 15 to 19 mass percent of MgO, mixing and reacting with 700 to 1,300 parts of byproduct of the purification of wet-process phosphoric acid, namely the raffinate which contains 42 to 46 mass percent of P2O5 and 3 to 6 mass percent of MgO in a reactor, and adding 0.1002 to 1.002 parts of surfactant, wherein the reaction time is 10 to 20min, and the reaction temperature is controlled to be between 40 and 60 DEG C; drying a fresh phosphorus-magnesium compound fertilizer obtained after the reaction at the temperature of 100+/-5 DEG C; and crushing and directly packaging to obtain a powdered phosphorus-magnesium compound fertilizer product. By the method, the resource of raw materials is wide, energy consumption is low, production period is short, and the quality of the product is reliable.
Description
Technical field
The invention belongs to the chemical fertilizers production technical field, relating to a kind of specifically is the method for feedstock production phosphorus magnesium compound fertilizer material with wet phosphoric acid purifying by-product raffinate and high magnesium phosphor tail slag.
Background technology
A kind of method of purifying phosphoric acid is the purpose that reaches purifying with extraction agent phosphoric acid extraction from phosphoric acid by wet process, and the remaining acid in extraction back is called raffinate.Its main component: P
2O
542-46%, MgO 3-6%.Raffinate is recycled problem and all is considered to a technical difficult problem all the time, though have a lot about contained many foreign ions in the raffinate are carried out the purification and impurity removal reported in literature, but all fundamentally do not solve the utilization ratio problem of raffinate, mainly there is following problem in it: raffinate is the by product behind the wet phosphoric acid purifying, again it is carried out the secondary removal of impurities, it is inevitable very big that it removes incidental expense; Complicated component in the raffinate, foreign ion is many, is difficult to foreign ion is eliminated; When raffinate being carried out removal of impurities, will inevitably cause the P in the raffinate with some chemical processes
2O
5Concentration significantly reduces, and industrial value is little.Therefore, it is all little with viable economically property technically to improve the utilization ratio problem of raffinate from the angle of raffinate purification and impurity removal.
To be Rock Phosphate (72Min BPL) obtain byproduct behind the phosphorus concentrate by floating and enriching to high magnesium phosphorus mine tailing, and its main thing is white jade stone [Mg (CO mutually
3)
2] and fluorapatite [Ca
5F (PO
4)
3], its P
2O
5Content is 4-7%, and MgO content is 15-19%, belongs to high magnesium low-grade phosphorus ore.For a long time, ore deposit flotation mill production technique all is to adopt the way of selecting nature to build a dam and store up to the processing of phosphate rock floating mine tailing both at home and abroad, and storing up of a large amount of flotation phosphate mine tailings not only will take a large amount of land resources, also bring pollution, and have huge potential safety hazard environment.From the angle of resources circulation economic utilization, comprehensive utilizating research and the exploitation of carrying out the phosphate rock floating mine tailing have important practical significance.In recent years, though there is the technology of phosphorus comprehensive utilization of tailing to come out, fundamentally do not solve the problem of utilizing of high magnesium mine tailings after the flotation.
At Chinese patent publication number CN101367673, " utilizing phosphate rock floating by-product mine tailing directly to prepare the method for phosphor magnesium fertilizer " disclosed on 02 18th, 2009, detailed process is a raw material with flotation phosphate mine tailing slurry, control its water content 40-45%, directly carry out hybrid reaction with mixture of sulfuric phosphoric acid, 60-90 ℃ of temperature of reaction control, reaction times 30-60min, thus make powdery or granular complex fertilizer.This method is to the pre-treatment of phosphorus mine tailing slurry the time, and its water content is wayward, can make the slip liquid-solid ratio big, temperature of reaction height during the reaction of phosphorus mine tailing and mixture of sulfuric phosphoric acid in addition, and reaction times and slaking are long drying cycle, and products obtained therefrom available phosphorus, effective Mg content are low.Chinese patent publication number CN101618981, disclose on 01 06th, 2010 a kind of " utilizing the phosphorus mine tailing method of the high magnesium phosphor tail slag production of flotation by-product phosphorus magnesium compound fertilizer again ", detailed process is that the phosphorus mine tailing after pulverizing with oven dry is a raw material, directly carry out hybrid reaction with mixture of sulfuric phosphoric acid, reaction times 35～55min, temperature of reaction is at 50～80 ℃, thereby makes powdery or granular complex fertilizer.Temperature of reaction height when the phosphorus mine tailing was with the mixture of sulfuric phosphoric acid reaction when this method was not enough, long reaction time, products obtained therefrom available phosphorus, effective Mg content are lower.
At present, existing phosphorus magnesium compound fertilizer material is produced ubiquity and problems such as energy consumption height, cost height.
Summary of the invention
A kind of raw material sources that the objective of the invention is to overcome above-mentioned shortcoming and provide are wide, energy consumption is low, utilize raffinate and high magnesium phosphor tail slag with short production cycle, reliable product quality prepare the method for phosphorus magnesium compound fertilizer material.
A kind of method of utilizing raffinate and high magnesium phosphor tail slag to prepare phosphorus magnesium compound fertilizer material of the present invention may further comprise the steps:
(1) with 1001-1003 part P
2O
5Massfraction is that 4-7%, MgO massfraction are that the high magnesium phosphor tail slag oven dry of 15-19%, pulverizing back contain P with 700-1300 part
2O
5Massfraction is that 42-46%, MgO massfraction are 3-6% wet phosphoric acid purifying by-product raffinate hybrid reaction in reactor, and adds 0.1002-1.002 part tensio-active agent, and the reaction times is 10-20min, and temperature of reaction is controlled at 40-60 ℃;
(2) will react the fresh phosphorus magnesium compound fertilizer material of back gained 100 ± 5 ℃ of oven dry down;
(3) just obtain powdery phosphorus magnesium compound fertilizer material product through pulverizing directly after the packing.
Above-mentioned a kind of method of utilizing raffinate and high magnesium phosphor tail slag to prepare phosphorus magnesium compound fertilizer material, wherein: tensio-active agent is Sodium dodecylbenzene sulfonate, AES etc.
Above-mentioned a kind of method of utilizing raffinate and high magnesium phosphor tail slag to prepare phosphorus magnesium compound fertilizer material, wherein: the phosphorus magnesium compound fertilizer material after will pulverizing adds water granulation on granulating disc, makes granular phosphorus magnesium compound fertilizer material after drying, the screening.
The present invention compared with prior art, has tangible beneficial effect, as can be known from the above technical solutions, adopting wet phosphoric acid purifying by-product raffinate and high magnesium phosphor tail slag is the direct hybrid reaction of raw material, and add a spot of tensio-active agent (Sodium dodecylbenzene sulfonate, AES etc.), help improving the rate of decomposition of high magnesium phosphorus mine tailing.Its P
2O
5Transformation efficiency more than 90%, the transformation efficiency of MgO is more than 85%.The present invention with wet phosphoric acid purifying after MgO and P in by-product raffinate and the high magnesium phosphor tail slag
2O
5Being converted into chemical fertilizer, can either effecting a radical cure the pollution problem of phosphor tail slag, improve the raffinate utilization ratio, it is turned waste into wealth, is again the effective way that improves the comprehensive utilization of resources rate.To guaranteeing that agricultural development and phosphorous chemical industry Sustainable development have important practical significance.Raw material sources of the present invention are wide, energy consumption is low, with short production cycle, reliable product quality, and the product of the phosphorus magnesium compound fertilizer material of being produced is by weight percentage: total phosphorus P
2O
528-36%, available phosphorus P
2O
523-33%, total magnesium MgO 14-16%, effectively magnesium MgO 9-11%, with P
2O
5Free acid≤5% of meter.
Embodiment
Embodiment 1:
Raw material:
1) raffinate: w (P
2O
5) 46.0%, w (MgO) 3.0%;
2) phosphor tail slag: w (P
2O
5) 5.5%, w (MgO) 16.2%.
High magnesium phosphor tail slag after by-product raffinate and 1001g oven dry is pulverized behind the 1000g wet phosphoric acid purifying joins and carries out the acidifying hybrid reaction in the reactive tank that has agitator, and interpolation 1.002g tensio-active agent Sodium dodecylbenzene sulfonate, control reaction temperature is 40 ℃ in the reaction process, reaction times 20min, after reaction finishes material drawn off and put into porcelain dish, dry cool to room temperature down at 100 ± 5 ℃, material is done solid and sclerosis, with its grinding and processing powdering phosphorus magnesium compound fertilizer material product.Powder is agglomerated into grain by adding water on granulating disc, drying, and particle diameter 1mm-4mm is being sieved in cooling, is granular phosphorus magnesium compound fertilizer material product.The product quality analysis result is as follows:
Embodiment 2
Raw material:
1) raffinate: w (P
2O
5) 44.6%, w (MgO) 5.4%;
2) phosphor tail slag: w (P
2O
5) 7.0%, w (MgO) 19.0%.
High magnesium phosphor tail slag after by-product raffinate and 1002g oven dry is pulverized behind the 1202g wet phosphoric acid purifying joins and carries out the acidifying hybrid reaction in the reactive tank that has agitator, and interpolation 0.1002g tensio-active agent Sodium dodecylbenzene sulfonate, control reaction temperature is 50 ℃ in the reaction process, reaction times 15min, after reaction finishes material drawn off and put into porcelain dish, dry cool to room temperature down at 100 ± 5 ℃, material is done solid and sclerosis, with its grinding and processing powdering phosphorus magnesium compound fertilizer material product.Powder is agglomerated into grain by adding water on granulating disc, drying, and particle diameter 1mm-4mm is being sieved in cooling, is granular phosphorus magnesium compound fertilizer material product.The product quality analysis result is as follows:
Embodiment 3
Raw material:
1) raffinate: w (P
2O
5) 44.1%, w (MgO) 6.0%;
2) phosphor tail slag: (P
2O
5) 5.4%, w (MgO) 17.2%.
High magnesium phosphor tail slag after by-product raffinate and 1003g oven dry is pulverized behind the 1300g wet phosphoric acid purifying joins and carries out the acidifying hybrid reaction in the reactive tank that has agitator, and the surfactant A ES of interpolation 0.1003g, control reaction temperature is 45 ℃ in the reaction process, reaction times 10min, after reaction finishes material drawn off and put into porcelain dish, dry cool to room temperature down at 100 ± 5 ℃, material is done solid and sclerosis, with its grinding and processing powdering phosphorus magnesium compound fertilizer material product.Powder is agglomerated into grain by adding water on granulating disc, drying, and particle diameter 1mm-4mm is being sieved in cooling, is granular phosphorus magnesium compound fertilizer material product.The product quality analysis result is as follows:
Embodiment 4
Raw material:
1) raffinate: w (P
2O
5) 42.0%, w (MgO) 4.8%;
2) phosphor tail slag: (P
2O
5) 4.0%, w (MgO) 15.0%.
High magnesium phosphor tail slag after by-product raffinate and 1003g oven dry is pulverized behind the 700g wet phosphoric acid purifying joins and carries out the acidifying hybrid reaction in the reactive tank that has agitator, and interpolation 1.003g surfactant A ES, control reaction temperature is 60 ℃ in the reaction process, reaction times 10min, after reaction finishes material drawn off and put into porcelain dish, dry cool to room temperature down at 100 ± 5 ℃, material is done solid and sclerosis, with its grinding and processing powdering phosphorus magnesium compound fertilizer material product.Powder is agglomerated into grain by adding water on granulating disc, drying, and particle diameter 1mm-4mm is being sieved in cooling, is granular phosphorus magnesium compound fertilizer material product.The product quality analysis result is as follows:
The above, it only is preferred embodiment of the present invention, be not that the present invention is done any pro forma restriction, any technical solution of the present invention content that do not break away from,, all still belong in the scope of technical solution of the present invention any simple modification, equivalent variations and modification that above embodiment did according to technical spirit of the present invention.
Claims (3)
1. method of utilizing raffinate and high magnesium phosphor tail slag to prepare phosphorus magnesium compound fertilizer material may further comprise the steps:
(1) with 1001-1003 part P
2O
5Massfraction is that 4-7%, MgO massfraction are that the high magnesium phosphor tail slag oven dry of 15-19%, pulverizing back contain P with 700-1300 part
2O
5Massfraction is that 42-46%, MgO massfraction are 3-6% wet phosphoric acid purifying by-product raffinate hybrid reaction in reactor, and adds 0.1002-1.002 part tensio-active agent, and the reaction times is 10-20min, and temperature of reaction is controlled at 40-60 ℃;
(2) will react the fresh phosphorus magnesium compound fertilizer material of back gained 100 ± 5 ℃ of oven dry down;
(3) just obtain powdery phosphorus magnesium compound fertilizer material product through pulverizing directly after the packing.
2. a kind of method of utilizing raffinate and high magnesium phosphor tail slag to prepare phosphorus magnesium compound fertilizer material as claimed in claim 1, wherein: tensio-active agent is Sodium dodecylbenzene sulfonate, AES.
3. a kind of method of utilizing raffinate and high magnesium phosphor tail slag to prepare phosphorus magnesium compound fertilizer material as claimed in claim 1 or 2; wherein: the phosphorus magnesium compound fertilizer material after will pulverizing adds water granulation on granulating disc, makes granular phosphorus magnesium compound fertilizer material after drying, the screening.
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| CN201010608653.XA CN102161602B (en) | 2010-12-28 | 2010-12-28 | Method for preparing phosphorus-magnesium compound fertilizer by utilizing raffinate and phosphate tailings with high magnesium content |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102924158A (en) * | 2012-12-01 | 2013-02-13 | 中化化肥有限公司重庆磷复肥工程技术研究中心 | Method for producing multielement nitro-compound fertilizer |
| CN103113139A (en) * | 2013-03-05 | 2013-05-22 | 中化化肥有限公司重庆磷复肥工程技术研究中心 | Method for producing multivariate nitro compound fertilizer from wet-process phosphoric acid purification sludge |
| CN104328481A (en) * | 2014-10-14 | 2015-02-04 | 瓮福（集团）有限责任公司 | Method for preparing gypsum whisker by using phosphate tailings and raffinate phosphoric acid |
| CN104387121A (en) * | 2014-11-10 | 2015-03-04 | 瓮福（集团）有限责任公司 | Method for preparing phosphorus-magnesium fertilizer |
| CN108456007A (en) * | 2018-04-02 | 2018-08-28 | 金正大生态工程集团股份有限公司 | A kind of calcium polyphosphate magnesium fertilizer and preparation method thereof prepared as raw material using phosphoric acid and phosphorus tailing |
| CN113277885A (en) * | 2021-06-09 | 2021-08-20 | 四川大学 | Resource utilization method of phosphoric acid residues |
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| CN1034913A (en) * | 1988-02-10 | 1989-08-23 | 成都科技大学 | With in the low-grade high-magnesium-phosphorus ore method of producing the ammonium magnesium-phosphorus fertilizer |
| CN101613094A (en) * | 2009-07-24 | 2009-12-30 | 瓮福（集团）有限责任公司 | Method with the raffinate production diammonium phosphate of purifying phosphoric acid |
| CN101618981A (en) * | 2009-07-28 | 2010-01-06 | 瓮福（集团）有限责任公司 | Method for producing phosphorus-magnesium compound fertilizer by using phosphate spoil-reclaiming byproduct high-magnesia tailing slag |
| CN101723731A (en) * | 2009-02-25 | 2010-06-09 | 山东三方化工集团有限公司 | Environment-friendly long-acting compound fertilizer and preparation method thereof |
| CN101891504A (en) * | 2010-07-26 | 2010-11-24 | 瓮福（集团）有限责任公司 | Method for producing granular monoammonium phosphate with raffinate |
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2010
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1034913A (en) * | 1988-02-10 | 1989-08-23 | 成都科技大学 | With in the low-grade high-magnesium-phosphorus ore method of producing the ammonium magnesium-phosphorus fertilizer |
| CN101723731A (en) * | 2009-02-25 | 2010-06-09 | 山东三方化工集团有限公司 | Environment-friendly long-acting compound fertilizer and preparation method thereof |
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| CN101618981A (en) * | 2009-07-28 | 2010-01-06 | 瓮福（集团）有限责任公司 | Method for producing phosphorus-magnesium compound fertilizer by using phosphate spoil-reclaiming byproduct high-magnesia tailing slag |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102924158A (en) * | 2012-12-01 | 2013-02-13 | 中化化肥有限公司重庆磷复肥工程技术研究中心 | Method for producing multielement nitro-compound fertilizer |
| CN103113139A (en) * | 2013-03-05 | 2013-05-22 | 中化化肥有限公司重庆磷复肥工程技术研究中心 | Method for producing multivariate nitro compound fertilizer from wet-process phosphoric acid purification sludge |
| CN103113139B (en) * | 2013-03-05 | 2015-02-04 | 中化化肥有限公司重庆磷复肥工程技术研究中心 | Method for producing multivariate nitro compound fertilizer from wet-process phosphoric acid purification sludge |
| CN104328481A (en) * | 2014-10-14 | 2015-02-04 | 瓮福（集团）有限责任公司 | Method for preparing gypsum whisker by using phosphate tailings and raffinate phosphoric acid |
| CN104387121A (en) * | 2014-11-10 | 2015-03-04 | 瓮福（集团）有限责任公司 | Method for preparing phosphorus-magnesium fertilizer |
| CN104387121B (en) * | 2014-11-10 | 2017-03-08 | 瓮福（集团）有限责任公司 | A kind of method preparing phosphorus fertiliser containing magnesium |
| CN108456007A (en) * | 2018-04-02 | 2018-08-28 | 金正大生态工程集团股份有限公司 | A kind of calcium polyphosphate magnesium fertilizer and preparation method thereof prepared as raw material using phosphoric acid and phosphorus tailing |
| WO2019192328A1 (en) | 2018-04-02 | 2019-10-10 | 金正大诺泰尔化学有限公司 | Polyphosphoric acid calcium magnesium fertilizer, polyphosphoric acid calcium magnesium fertilizer prepared by using phosphoric acid and phosphorus tailings as raw materials and preparation method therefor |
| CN108456007B (en) * | 2018-04-02 | 2021-05-25 | 金正大生态工程集团股份有限公司 | Calcium-magnesium polyphosphate fertilizer prepared by taking phosphoric acid and phosphate tailings as raw materials and preparation method thereof |
| US11787748B2 (en) | 2018-04-02 | 2023-10-17 | Kingenta Ecological Engineering Group Co., Ltd. | Polyphosphoric acid calcium magnesium fertilizer, polyphosphoric acid calcium magnesium fertilizer prepared by using phosphoric acid and phosphorus tailings as raw material and preparation method therefor |
| CN113277885A (en) * | 2021-06-09 | 2021-08-20 | 四川大学 | Resource utilization method of phosphoric acid residues |
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