CN106187550A - A kind of method utilizing red mud flocculation agent acid leaching residue to prepare siliceous fertilizer - Google Patents
A kind of method utilizing red mud flocculation agent acid leaching residue to prepare siliceous fertilizer Download PDFInfo
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- CN106187550A CN106187550A CN201610619266.3A CN201610619266A CN106187550A CN 106187550 A CN106187550 A CN 106187550A CN 201610619266 A CN201610619266 A CN 201610619266A CN 106187550 A CN106187550 A CN 106187550A
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- red mud
- acid leaching
- leaching residue
- flocculation agent
- agent acid
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
- C05D1/00—Fertilisers containing potassium
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
- C05D9/00—Other inorganic fertilisers
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- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Pest Control & Pesticides (AREA)
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Abstract
The invention discloses a kind of method utilizing red mud flocculation agent acid leaching residue to prepare siliceous fertilizer, belong to agricultural fertilizer preparing technical field.The present invention, with red mud flocculation agent acid leaching residue as raw material, comprises the steps of 1) pretreatment red mud flocculation agent acid leaching residue；2) red mud flocculation agent acid leaching residue obtained in the previous step is mixed in proportion with potassium hydroxide and potassium carbonate；3) after previous step being mixed material calcining, cooling, levigate；4) sample levigate for previous step is added appropriate synergist, and add appropriate water, i.e. can obtain meeting the siliceous fertilizer of national standard.The present invention compensate for preparing the blank of siliceous fertilizer research with red mud flocculation agent acid leaching residue, and preparation method facilitates convenient, and raw material sources are extensive, production cost is low, applied range, the siliceous fertilizer produced has significant effect to growth and the volume increase of plant, meets environmental protection theory.
Description
Technical field
The invention belongs to agricultural fertilizer preparing technical field, be specifically related to one and utilize red mud flocculation agent acid leaching residue to prepare silicon
Fertile method.
Background technology
Siliceous fertilizer, belongs to a kind of secondary nutrients.Siliceous fertilizer by international soil circle be classified as after nitrogen, phosphorus, potassium the fourth-largest
Element fertilizer.Whether country's soil measurement formula using lacking silicon dioxide as technical standard, and on June 1st, 2004, the Ministry of Agriculture promulgates
The siliceous fertilizer industry standard NY/T 797-2004 that completed by units such as China Agriculture Academe Fertilizer Institute, indicates
Through years of researches test and popularization, siliceous fertilizer has become a kind of new-type fertilizer of 21 century China.
At present, China lacks tripoli earth and accounts for more than the 50 ~ 80% of total area under cultivation, as a example by Oryza sativa L., and the long-term rice cultivation of China
Area reach more than 3,333 ten thousand hectares, lack tripoli earth account for more than 50%.If all Applying silicon fertilizers, based on volume increase 10%, only this item
Should increase production 1,000,000 tons of Oryza glutinosa every year, the production promoting siliceous fertilizer has obviously Social and economic benef@with application.
The kind of siliceous fertilizer mainly has solubility in citric acid siliceous fertilizer, the big class of Water-soluble silicon fertilizer two, solubility in citric acid siliceous fertilizer refer to water insoluble and
The siliceous fertilizer can being absorbed by plants after being dissolved in acid, common mostly is the steel slag of steel mill, flyash, Ore through high-temperature calcination work
Skills etc. process, and general amount of application is relatively big (every mu about 25-50 kilogram), is suitable for doing soil base and executes, and market price is relatively low (every
The hundreds of unit of ton is to thousands of units)；Water-soluble silicon fertilizer refers to be dissolved in the siliceous fertilizer that water directly can be absorbed by plant, and crops are to it
Absorption rate is higher, synthesizes for high temeperature chemistry, and production technology is more complicated, relatively costly, but amount of application is less, is typically commonly used for
Foliage-spray, punching are executed and drip irrigation, it is possible to carry out Ji Shi and impose, and concrete consumption can be according to crop varieties happiness silicon situation, local soil
Depending on the scarce silicon situation of earth and the concrete content of siliceous fertilizer.
China is the first in the world big alumina producing state and country of consumption, and yield accounts for the 39% of whole world total output, and consumption figure accounts for generation
The 45% of boundary's consumption figure.Red mud is the contaminative waste residue discharged during aluminium industry extraction aluminium oxide, and average often produces 1 ton of oxygen
Change aluminum, incidentally produce 1.0～2.0 tons of red muds.China is as alumina producing state the biggest in the world, the most built the biggest in the world
Aluminum oxide industry system, produces red mud about 70,000,000 tons in year.
Red mud mineralogical composition is complicated, and its essential mineral is serpentine and calcite, and content is 60% ~ 65%, next to that albumen
Stone, gibbsite, goethitum, what content was minimum is titanium ore, siderite, trona, waterglass, sodium aluminate and Caustic soda.Its ore deposit
Thing complicated component, and do not meet the mineral assemblage of natural earth.Being analyzed its chemical composition, result shows, its aluminium oxide, oxygen
Change iron content general all about 25%, therefore its raw material that can be used as aluminium polychlorid and poly-ferric chloride utilizes hydrochloric acid
The red mud flocculation agent acid leaching residue that acidleach red mud obtains, patent inventor has carried out substantial amounts of research to it, its master of preliminary analysis
Want composition as follows:
Shandong Wei Qiao alumina producer red mud flocculation agent acid leaching residue main chemical compositions
| Composition | SiO2 | Al2O3 | CaO | Fe2O3 | TiO2 | K2O | MgO | Cl |
| Content/% | 40.63 | 20.10 | 1.47 | 9.9 | 9.18 | 0.275 | 0.245 | 1.87 |
Owing to red mud flocculation agent acid leaching residue acidity is high, at present almost without being applied, subsoil water, periphery are planted by substantial amounts of accumulation
Quilt and air cause substantial amounts of harm.Through consulting literatures, have red mud flocculation agent acid almost without researcher and mechanism at present
Leaching slag carries out research on utilization.Inventor, for red mud flocculation agent acid leaching residue, utilizes its specific character, by washing and activation
Agent mixed calcining, mediates pelletize, prepares a kind of red mud flocculation agent acid leaching residue siliceous fertilizer.This patent not only avoid red mud flocculation agent
The acid leaching residue pollution to environment, is made into fertilizer, furthermore achieved that its recycling.
Summary of the invention
It is an object of the invention to provide a kind of method utilizing red mud flocculation agent acid leaching residue to prepare siliceous fertilizer, raw material easily obtains
Obtain, can be mass-produced and low cost.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of method utilizing red mud flocculation agent acid leaching residue to prepare siliceous fertilizer, comprises the following steps:
(1) red mud flocculation agent acid leaching residue is carried out pretreatment；
(2) the red mud flocculation agent acid leaching residue after the first step being processed is mixed homogeneously with potassium hydroxide and potassium carbonate；
(3) raw material of second step mix homogeneously is calcined, afterwards cooling, levigate；
(4) raw material after levigate for the 3rd step is added synergist, make up water and stir, utilize granulator granulation, dry, i.e.
Available siliceous fertilizer.
Preferably, in step (1), the method for pretreatment is: be (1 ~ 2) in mass ratio with water by red mud flocculation agent acid leaching residue:
(3 ~ 5) mix, and stir, and after settling 15 ~ 30 hours, take off a layer solid sediment, and 80 ~ 120 DEG C are dried, levigate.Red mud
Flocculant acid leaching residue water-washing pre-treatment part is to remove the hydrochloric acid of excess in red mud flocculation agent acid leaching residue, making red mud flocculation agent
The pH value of acid leaching residue is increased to about 3 by about 0, another purpose be in order to remove as far as possible in red mud flocculation agent acid leaching residue for
The invalid components such as compositions such as sodium chloride, iron chloride and aluminum chloride such as the inorganic salt preparing siliceous fertilizer.
Preferably, in parts by weight, in step (2), the proportioning raw materials of each component is: red mud flocculation agent acid leaching residue 40 ~
70 parts, potassium hydroxide 20 ~ 30 parts, potassium carbonate 5 ~ 15 parts.Experimental design utilizes the red mud flocculation agent acid of potassium hydroxide and pretreatment
In leaching slag, insoluble silicon dioxide reacts, and generates the soluble silicates such as potassium silicate, thus improves its available silicon content.Carbon
The addition of acid potassium is that potassium carbonate at high temperature decomposes in order to reduce while production cost, produces carbon dioxide, can make finally to calcine
Afterproduct is loose porous, and specific surface area increases, and improves its reactivity further, thus plays the effect of potentiation.
Preferably, the raw material mixed being placed in Muffle furnace in step (3) calcining, calcining heat is 350 ~ 500 DEG C, forges
The burning time is 3 ~ 8 hours.
Preferably, in parts by weight, the synergist in step (4) is 2 ~ 5 parts of waterglass, adds through abovementioned steps
Prepared sample quality is the water of 5 ~ 10%, carries out pelletize in roller pelletizer, controls balling-up granularity at 5 ~ 10mm, then 100 ~
130 DEG C of drying, i.e. obtain siliceous fertilizer prepared by red mud flocculation agent acid leaching residue.Waterglass itself is a kind of well Water-soluble silicon fertilizer,
It is also a kind of well viscosifier simultaneously, and it is that a part can improve having of the siliceous fertilizer of preparation that this part adds the reason of waterglass
The content of effect silicon, another portion its can improve the viscosity of last composite granule, improve pelletize rate.
Advantages of the present invention: had without scientific research institution and scholar the most temporarily and utilize red mud flocculation agent acid leaching residue to prepare siliceous fertilizer work
Skill report and research, the present invention compensate for the blank of this part, and inventor effectively make use of red mud flocculation agent acid leaching residue, belongs to
Resource recycling technology, meets the requirement of environmental protection, and Productive statistics is low, has bigger industrial value, can be prevented effectively from
Environmental pollution.
Detailed description of the invention
Embodiment 1:
(1) by red mud flocculation agent acid leaching residue 20kg, water 60kg, stir, after settling 24 hours, take off a layer solid sediment,
105 DEG C be dried, levigate processed after red mud flocculation agent acid leaching residue；
(2) red mud flocculation agent acid leaching residue after the process that will obtain in (1), potassium hydroxide, potassium carbonate are respectively as follows: red mud by quality
Flocculant acid leaching residue 6kg, potassium hydroxide 3kg, potassium carbonate 1.5kg mix homogeneously；
(3) by the sample that obtains in (2) in Muffle furnace 400 DEG C calcine 4 hours, cooling, levigate；
(4) the levigate material obtained in (3) is added the waterglass of 0.5kg, adds the water of 0.5kg, enter in roller pelletizer
Row pelletize, control balling-up granularity between 5 ~ 10mm, the silicon that then 120 DEG C of drying are prepared to red mud flocculation agent acid leaching residue
Fertile.
The siliceous fertilizer of preparation uses hexafluosilicic acid in People's Republic of China's agricultural industry criteria NY/T 797-2004 siliceous fertilizer standard
Potassium capacity method is measured, available silicon content 24.32%, moisture 1.6%, fineness (by 250 μm standard screens) 88%.Reach NY/T
797-2004 siliceous fertilizer standard: available silicon content >=20%, moisture≤3%, fineness (by 250 μm standard screens) >=80%.
Embodiment 2:
(1) by red mud flocculation agent acid leaching residue 20kg, water 60kg, stir, after settling 24 hours, take off a layer solid sediment,
80 DEG C be dried, levigate processed after red mud flocculation agent acid leaching residue；
(2) red mud flocculation agent acid leaching residue after the process that will obtain in (1), potassium hydroxide, potassium carbonate are respectively as follows: red mud by quality
Flocculant acid leaching residue 4kg, potassium hydroxide 2kg, potassium carbonate 0.5kg mix homogeneously；
(3) by the sample that obtains in (2) in Muffle furnace 350 DEG C calcine 4 hours, cooling, levigate；
(4) the levigate material obtained in (3) is added the waterglass of 0.2kg, adds the water of 0.5kg, enter in roller pelletizer
Row pelletize, controls balling-up granularity at 5 ~ 10mm, the siliceous fertilizer that then 100 DEG C of drying are prepared to red mud flocculation agent acid leaching residue.
The siliceous fertilizer of preparation uses hexafluosilicic acid in People's Republic of China's agricultural industry criteria NY/T 797-2004 siliceous fertilizer standard
Potassium capacity method is measured, available silicon content 23.3%, moisture 2.9%, fineness (by 250 μm standard screens) 82%.Reach NY/T
797-2004 siliceous fertilizer standard: available silicon content >=20%, moisture≤3%, fineness (by 250 μm standard screens) >=80%.
Embodiment 3:
(1) by red mud flocculation agent acid leaching residue 30kg, water 80kg, stir, after settling 24 hours, take off a layer solid sediment,
105 DEG C be dried, levigate processed after red mud flocculation agent acid leaching residue；
(2) red mud flocculation agent acid leaching residue after the process that will obtain in (1), potassium hydroxide, potassium carbonate are respectively as follows: red mud by quality
Flocculant acid leaching residue 6kg, potassium hydroxide 2.5kg, potassium carbonate 1kg mix homogeneously；
(3) by the sample that obtains in (2) in Muffle furnace 400 DEG C calcine 4 hours, cooling, levigate；
(4) the levigate material obtained in (3) is added the waterglass of 0.3kg, adds the water of 0.7kg, enter in roller pelletizer
Row pelletize, control balling-up granularity between 5 ~ 10mm, the silicon that then 120 DEG C of drying are prepared to red mud flocculation agent acid leaching residue
Fertile.
The siliceous fertilizer of preparation uses hexafluosilicic acid in People's Republic of China's agricultural industry criteria NY/T 797-2004 siliceous fertilizer standard
Potassium capacity method is measured, available silicon content 21.3%, moisture 2.1%, fineness (by 250 μm standard screens) 85%.Reach NY/T
797-2004 siliceous fertilizer standard: available silicon content >=20%, moisture≤3%, fineness (by 250 μm standard screens) >=80%.
Embodiment 4:
(1) by red mud flocculation agent acid leaching residue 40kg, water 100kg, stir, after settling 24 hours, take off a layer solid sediment,
120 DEG C be dried, levigate processed after red mud flocculation agent acid leaching residue；
(2) red mud flocculation agent acid leaching residue after the process that will obtain in (1), potassium hydroxide, potassium carbonate are respectively as follows: red mud by quality
Flocculant acid leaching residue 7kg, potassium hydroxide 3kg, potassium carbonate 1.5kg mix homogeneously；
(3) by the sample that obtains in (2) in Muffle furnace 500 DEG C calcine 4 hours, cooling, levigate；
(4) the levigate material obtained in (3) is added the waterglass of 0.5kg, adds the water of 1kg, carry out in roller pelletizer
Pelletize, controls balling-up granularity at 5 ~ 10mm, the siliceous fertilizer that then 120 DEG C of drying are prepared to red mud flocculation agent acid leaching residue.
The siliceous fertilizer of preparation uses hexafluosilicic acid in People's Republic of China's agricultural industry criteria NY/T 797-2004 siliceous fertilizer standard
Potassium capacity method is measured, available silicon content 20.3%, moisture 1.8%, fineness (by 250 μm standard screens) 86%.Reach NY/T
797-2004 siliceous fertilizer standard: available silicon content >=20%, moisture≤3%, fineness (by 250 μm standard screens) >=80%.
Comparative example:
(1) by red mud flocculation agent acid leaching residue 10kg, water 60kg, stir, after settling 24 hours, take off a layer solid sediment,
105 DEG C be dried, levigate processed after red mud flocculation agent acid leaching residue；
(2) red mud flocculation agent acid leaching residue after the process that will obtain in (1), potassium hydroxide, potassium carbonate are respectively as follows: red mud by quality
Flocculant acid leaching residue 3kg, potassium hydroxide 1kg, potassium carbonate 0.3kg mix homogeneously；By the sample that obtains in (2) in Muffle furnace
300 DEG C calcine 4 hours, cooling, levigate；
(3) the levigate material obtained in (3) is added the waterglass of 0.3kg, adds the water of 0.7kg, enter in roller pelletizer
Row pelletize, controls balling-up granularity at 5 ~ 10mm, the siliceous fertilizer that then 120 DEG C of drying are prepared to red mud flocculation agent acid leaching residue.
The siliceous fertilizer of preparation uses hexafluosilicic acid in People's Republic of China's agricultural industry criteria NY/T 797-2004 siliceous fertilizer standard
Potassium capacity method is measured, available silicon content 7.3%, moisture 1.8%, fineness (by 250 μm standard screens) 81%.It is not up to NY/T
797-2004 siliceous fertilizer standard: available silicon content >=20%, moisture≤3%, fineness (by 250 μm standard screens) >=80%.
Last it is noted that obviously, above-described embodiment is only for clearly demonstrating example of the present invention, and not
Restriction to embodiment.For those of ordinary skill in the field, can also make on the basis of the above description
The change of other multi-form or variation.Here without also cannot all of embodiment be given exhaustive.And thus amplified
Go out obviously changes or changes among still in protection scope of the present invention.
Claims (5)
1. one kind utilizes the method that red mud flocculation agent acid leaching residue prepares siliceous fertilizer, it is characterised in that comprise the following steps:
(1) red mud flocculation agent acid leaching residue is carried out pretreatment；
(2) the red mud flocculation agent acid leaching residue after the first step being processed is mixed homogeneously with potassium hydroxide and potassium carbonate；
(3) raw material of second step mix homogeneously is calcined, afterwards cooling, levigate；
(4) raw material after levigate for the 3rd step is added synergist, makes up water and stir, utilize granulator granulation, dry,
Obtain siliceous fertilizer.
A kind of method utilizing red mud flocculation agent acid leaching residue to prepare siliceous fertilizer, it is characterised in that step
(1) in, the method for pretreatment is: by red mud flocculation agent acid leaching residue with water in mass ratio for (1 ~ 2): (3 ~ 5) mix, and stir all
Even, after settling 15 ~ 30 hours, take off a layer solid sediment, 80 ~ 120 DEG C are dried, levigate.
A kind of method utilizing red mud flocculation agent acid leaching residue to prepare siliceous fertilizer, it is characterised in that according to
Parts by weight meter, in step (2), the proportioning raw materials of each component is: red mud flocculation agent acid leaching residue 40 ~ 70 parts, potassium hydroxide 20 ~ 30
Part, potassium carbonate 5 ~ 15 parts.
A kind of method utilizing red mud flocculation agent acid leaching residue to prepare siliceous fertilizer, it is characterised in that step
(3) raw material mixed is placed in Muffle furnace in calcining, and calcining heat is 350 ~ 500 DEG C, and calcination time is 3 ~ 8 hours.
A kind of method utilizing red mud flocculation agent acid leaching residue to prepare siliceous fertilizer, it is characterised in that according to
Parts by weight meter, the synergist in step (4) is 2 ~ 5 parts of waterglass, and it is 5 ~ 10% that interpolation prepares sample quality through abovementioned steps
Water, roller pelletizer carries out pelletize, balling-up granularity is at 5 ~ 10mm, and then 100 ~ 130 DEG C of drying, i.e. obtain red mud flocculation
Siliceous fertilizer prepared by agent acid leaching residue.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107141172A (en) * | 2017-05-19 | 2017-09-08 | 中国地质大学（北京） | A kind of method that utilization Leaching Metals from Red mud slag prepares composite mineral fertilizer with shepardite sintering |
| CN108610098A (en) * | 2016-12-12 | 2018-10-02 | 贵州远盛钾业科技有限公司 | A kind of production method of water-soluble silicon-potassium fertilizer material |
| CN111690810A (en) * | 2019-03-12 | 2020-09-22 | 中南大学 | Red mud recycling-soil treatment method |
| WO2022227181A1 (en) * | 2021-04-28 | 2022-11-03 | 东北大学 | Method for preparing silicon-potassium-calcium compound fertilizer by using calcium-containing red mud |
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| CN101440324A (en) * | 2008-12-24 | 2009-05-27 | 贵州平坝宏大铝化工有限公司 | Comprehensive utilization of Bayer process red mud |
| CN103924068A (en) * | 2013-01-14 | 2014-07-16 | 中国地质大学（北京） | Pellet binder based on red mud and iron-bearing minerals, and preparation method thereof |
| CN103922448A (en) * | 2013-01-14 | 2014-07-16 | 中国地质大学（北京） | Method for preparing multi-component flocculant and co-producing composite white carbon black by using red mud |
| CN104119161A (en) * | 2014-08-12 | 2014-10-29 | 许盛英 | Method for producing red mud compressed nutrient soil |
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| CN101440324A (en) * | 2008-12-24 | 2009-05-27 | 贵州平坝宏大铝化工有限公司 | Comprehensive utilization of Bayer process red mud |
| CN103924068A (en) * | 2013-01-14 | 2014-07-16 | 中国地质大学（北京） | Pellet binder based on red mud and iron-bearing minerals, and preparation method thereof |
| CN103922448A (en) * | 2013-01-14 | 2014-07-16 | 中国地质大学（北京） | Method for preparing multi-component flocculant and co-producing composite white carbon black by using red mud |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108610098A (en) * | 2016-12-12 | 2018-10-02 | 贵州远盛钾业科技有限公司 | A kind of production method of water-soluble silicon-potassium fertilizer material |
| CN107141172A (en) * | 2017-05-19 | 2017-09-08 | 中国地质大学（北京） | A kind of method that utilization Leaching Metals from Red mud slag prepares composite mineral fertilizer with shepardite sintering |
| CN107141172B (en) * | 2017-05-19 | 2020-06-02 | 中国地质大学（北京） | Method for preparing mineral compound fertilizer by sintering red mud acid leaching residue and brucite |
| CN111690810A (en) * | 2019-03-12 | 2020-09-22 | 中南大学 | Red mud recycling-soil treatment method |
| CN111690810B (en) * | 2019-03-12 | 2021-08-27 | 中南大学 | Red mud recycling-soil treatment method |
| WO2022227181A1 (en) * | 2021-04-28 | 2022-11-03 | 东北大学 | Method for preparing silicon-potassium-calcium compound fertilizer by using calcium-containing red mud |
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