CN102030566B - New process for producing efficient calcium magnesium sulphur silicon fertilizer by utilizing slag from magnesium reduction furnace - Google Patents
New process for producing efficient calcium magnesium sulphur silicon fertilizer by utilizing slag from magnesium reduction furnace Download PDFInfo
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- CN102030566B CN102030566B CN2010105537039A CN201010553703A CN102030566B CN 102030566 B CN102030566 B CN 102030566B CN 2010105537039 A CN2010105537039 A CN 2010105537039A CN 201010553703 A CN201010553703 A CN 201010553703A CN 102030566 B CN102030566 B CN 102030566B
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- Prior art keywords
- magnesium
- calcium
- reducing furnace
- furnace slag
- silicon fertilizer
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- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 47
- 239000011777 magnesium Substances 0.000 title claims abstract description 47
- 239000002893 slag Substances 0.000 title claims abstract description 46
- 239000003337 fertilizer Substances 0.000 title claims abstract description 23
- BNVZOJUDDYZFQY-UHFFFAOYSA-N [S].[Mg].[Ca].[Si] Chemical compound [S].[Mg].[Ca].[Si] BNVZOJUDDYZFQY-UHFFFAOYSA-N 0.000 title claims abstract description 12
- 238000000034 method Methods 0.000 title abstract description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 34
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 23
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000013078 crystal Substances 0.000 claims abstract description 19
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims abstract description 18
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 claims abstract description 18
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 17
- 229920000642 polymer Polymers 0.000 claims abstract description 16
- 239000001117 sulphuric acid Substances 0.000 claims abstract description 15
- 235000011149 sulphuric acid Nutrition 0.000 claims abstract description 15
- 238000004519 manufacturing process Methods 0.000 claims abstract description 12
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims abstract description 9
- 239000001110 calcium chloride Substances 0.000 claims abstract description 9
- 229910001628 calcium chloride Inorganic materials 0.000 claims abstract description 9
- 229910001629 magnesium chloride Inorganic materials 0.000 claims abstract description 9
- 238000001704 evaporation Methods 0.000 claims abstract description 7
- 238000002425 crystallisation Methods 0.000 claims description 10
- 230000008025 crystallization Effects 0.000 claims description 10
- AFYNYVFJTDCVBJ-UHFFFAOYSA-N [Si].[S] Chemical compound [Si].[S] AFYNYVFJTDCVBJ-UHFFFAOYSA-N 0.000 claims description 9
- ZFXVRMSLJDYJCH-UHFFFAOYSA-N calcium magnesium Chemical compound [Mg].[Ca] ZFXVRMSLJDYJCH-UHFFFAOYSA-N 0.000 claims description 9
- 238000000227 grinding Methods 0.000 claims description 9
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 9
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 9
- 230000008020 evaporation Effects 0.000 claims description 5
- 238000005469 granulation Methods 0.000 claims description 5
- 230000003179 granulation Effects 0.000 claims description 5
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 3
- 238000009837 dry grinding Methods 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 239000012467 final product Substances 0.000 claims description 2
- 238000003828 vacuum filtration Methods 0.000 claims description 2
- 238000001914 filtration Methods 0.000 abstract description 4
- 238000002156 mixing Methods 0.000 abstract description 4
- 239000002699 waste material Substances 0.000 abstract description 4
- 239000006227 byproduct Substances 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 abstract 4
- 235000012239 silicon dioxide Nutrition 0.000 abstract 3
- 229910052943 magnesium sulfate Inorganic materials 0.000 abstract 2
- 235000019341 magnesium sulphate Nutrition 0.000 abstract 2
- 239000002075 main ingredient Substances 0.000 abstract 1
- 238000005453 pelletization Methods 0.000 abstract 1
- 239000000843 powder Substances 0.000 abstract 1
- 230000008021 deposition Effects 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 239000011449 brick Substances 0.000 description 2
- 239000004568 cement Substances 0.000 description 2
- 235000003599 food sweetener Nutrition 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000003765 sweetening agent Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 241001558929 Sclerotium <basidiomycota> Species 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000006253 efflorescence Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 206010037844 rash Diseases 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000004901 spalling Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
The invention relates to a new process for producing efficient calcium magnesium sulphur silicon fertilizer by utilizing slag from a magnesium reduction furnace, which comprises the following steps of: firstly, crushing the slag from the magnesium reduction furnace to form about 100 to 200-mesh powder, reacting with diluted hydrochloric acid, and filtering out a silicon dioxide polymer; secondly, dividing filter liquor into two parts, evaporating and crystallizing one part directly to form mixed crystals of calcium chloride and magnesium chloride, and after reacting the other part with dilute sulphuric acid fully, evaporating and crystallizing to obtain mixed crystals of calcium sulfate and magnesium sulfate; and finally, mixing the silicon dioxide polymer and the all mixed crystals, and pelletizing to produce the calcium magnesium sulphur silicon fertilizer. In the new process, fertilizer of which the main ingredients are the calcium chloride, the magnesium chloride, the calcium sulfate, the magnesium sulfate, active silicon dioxide and the like is produced by taking industrial by-products such as the slag from the magnesium reduction furnace, the diluted hydrochloric acid, the dilute sulphuric acid and the like as raw materials, so the problems that the slag from the magnesium reduction furnace is difficult to process and the environment is polluted seriously are solved completely; and the new process has the advantages of turning waste into treasure along with low production cost, no secondary pollution and the like, and has wide market prospects.
Description
Technical field
The present invention relates to a kind of novel process, relate in particular to and utilize the magnesium reducing furnace slag to produce the novel process of calcium magnesium sulphur silicon fertilizer magnesium reducing furnace slag recycling.
Background technology
In the smelting process of MAGNESIUM METAL 99, can produce a large amount of magnesium reducing furnace slags, this waste residue is prone to efflorescence, and aquation solution shows alkalescence, serious environment pollution.Resource recycling mode for the magnesium reducing furnace slag mainly comprises at present: make Mg-slag brick, materials for wall, cement ingredient and sweetening agent etc.Because the MgO content in the magnesium reducing furnace slag is higher, and the composition less stable, causes the sclerotium spalling of Mg-slag brick, materials for wall and cement products easily, has limited the large-scale application of magnesium reducing furnace slag; And the magnesium reducing furnace slag is also at the experimental stage as the research of sweetening agent, and receive the restriction of industrial use aspect.Therefore the handling problem of magnesium reducing furnace slag can be described as the major obstacle of magnesium industry development.
Summary of the invention
The objective of the invention is to: a kind of novel process of utilizing the magnesium reducing furnace slag to produce calcium magnesium sulphur silicon fertilizer is provided.This technology is raw material with magnesium reducing furnace slag, industrial dilute hydrochloric acid and dilute sulphuric acid, and production can supply the calcium magnesium sulphur silicon fertilizer of crop absorption, turns waste into wealth, and makes that the magnesium reducing furnace slag is hard to manage, problem of environment pollution caused is solved.
Utilize the novel process of the efficient calcium magnesium of magnesium reducing furnace slag production sulphur silicon fertilizer, may further comprise the steps:
(1) with the magnesium reducing furnace slag through about pulverizer grinding to 100～200 orders;
(2) after magnesium reducing furnace slag behind the grinding and Hydrogen chloride fully react, filter out filter residue, promptly silica polymer is subsequent use with the silica polymer oven dry grinding that obtains;
(3) filtrating is divided into two parts of A, B; A, B ratio are 1: (1.7～2); After A solution and dilute sulphuric acid fully reacted, evaporative crystallization went out the mixed crystal of calcium sulfate and sal epsom, and B solution goes out to contain the mixed crystal of calcium chloride and magnesium chloride 100～150 ℃ of following direct evaporation crystallizations;
(4) mixed crystal of silica polymer, calcium chloride crystal and magnesium chloride, calcium sulfate and sal epsom mixed crystal are mixed the back granulation, get final product calcium magnesium sulphur silicon fertilizer.
The composition of the magnesium reducing furnace slag in the said step (1) is: CaO:45～58%, MgO:7～10%, SiO
2: 25～35%, Fe
2O
3: 4～5%, Al
2O
3Ignore.
The required Hydrogen chloride concentration of reaction is between 15～25% in the said step (2), reacts required dilute sulphuric acid concentration between 25～40%.
The proportional range of the required magnesium reducing furnace slag of the said novel process of utilizing the efficient calcium magnesium of magnesium reducing furnace slag production sulphur silicon fertilizer, Hydrogen chloride, dilute sulphuric acid is 1: (2～2.5): (1.5～2).
After will drying in the said step (2) silica polymer grinding to 100～200 orders.
Be to utilize vacuum filtration to leach filter residue in the said step (2).
The present invention has following several big advantage than the treatment process of other magnesium reducing furnace slag:
(1) China is large agricultural country, year makes fertilizer application amount very big, and China ploughs and generally lack elements such as calcium, magnesium, sulphur, silicon, therefore the magnesium reducing furnace slag is processed calcium magnesium sulphur silicon fertilizer, and market outlook are wide.
(2) required hydrochloric acid and the sulfuric acid of technology is industry byproduct, and production cost is low.
(3) technology is simple, and cost of investment is low.
(4) the magnesium reduction slag is thoroughly turned waste into wealth non-secondary pollution.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
Magnesium reducing furnace raw slag used in the present invention adopts the magnesium reduction slag of Wenxi County, Shanxi silver light magnesium industry company, and its chemical ingredients CaO is 57.5%, and MgO is 7.26%, SiO
2Be 30.5%, Fe
2O
3Be 4.18%, Al
2O
3Be 0.46%, all the other are impurity.
Embodiment 1:
With pulverizer the magnesium reducing furnace pulverized slag is milled to 100 orders, takes by weighing 100g, and prepare the hydrochloric acid 300mL of 15% concentration, the sulfuric acid 200mL of 30% concentration; The Hydrogen chloride of 15% concentration is slowly sneaked into the magnesium reducing furnace slag, constantly stir, reduce between 6～7 until the solution pH value; Use the vacuum pump filtering reacting solution, isolate silica polymer, oven dry back secondary grinding to 150 order; To filtrate is divided into two parts of A, B in the 1:1.7 ratio, in A solution, adds the dilute sulphuric acid of 30% concentration, does not have deposition generation continued and splashes into the dilute sulphuric acid about 30mL, and evaporative crystallization goes out the mixed crystal of calcium sulfate and sal epsom; At 150 ℃ of following direct evaporation B solution, go out the mixed crystal of calcium chloride and magnesium chloride until crystallization; With silica polymer and all xln mixing granulations, can obtain calcium magnesium sulphur silicon fertilizer at last.
Embodiment 2:
With pulverizer the magnesium reducing furnace pulverized slag is milled to 150 orders, takes by weighing 100g, and prepare the hydrochloric acid 300mL of 20% concentration, the sulfuric acid 200mL of 35% concentration; The Hydrogen chloride of 20% concentration is slowly sneaked into the magnesium reducing furnace slag, constantly stir, reduce between 6～7 until the solution pH value; Use the vacuum pump filtering reacting solution, isolate silica polymer, oven dry back secondary grinding to 150 order; To filtrate is divided into two parts of A, B in the 1:2 ratio, in A solution, adds the dilute sulphuric acid of 35% concentration, does not have deposition generation continued and splashes into the dilute sulphuric acid about 20mL, and evaporative crystallization goes out the mixed crystal of calcium sulfate and sal epsom; At 150 ℃ of following direct evaporation B solution, go out the mixed crystal of calcium chloride and magnesium chloride until crystallization; With silica polymer and all xln mixing granulations, can obtain calcium magnesium sulphur silicon fertilizer at last.
Embodiment 3:
With pulverizer the magnesium reducing furnace pulverized slag is milled to 200 orders, takes by weighing 100g, and prepare the hydrochloric acid 300mL of 25% concentration, the sulfuric acid 200mL of 40% concentration; The Hydrogen chloride of 25% concentration is slowly sneaked into the magnesium reducing furnace slag, constantly stir, reduce between 6～7 until the solution pH value; Use the vacuum pump filtering reacting solution, isolate silica polymer, oven dry back secondary grinding to 150 order; To filtrate is divided into two parts of A, B in the 1:2 ratio, in A solution, adds the dilute sulphuric acid of 40% concentration, does not have deposition generation continued and splashes into the dilute sulphuric acid about 10mL, and evaporative crystallization goes out the mixed crystal of calcium sulfate and sal epsom; At 150 ℃ of following direct evaporation B solution, go out the mixed crystal of calcium chloride and magnesium chloride until crystallization; With silica polymer and all xln mixing granulations, can obtain calcium magnesium sulphur silicon fertilizer at last.
Claims (5)
1. utilize the technology of the efficient calcium magnesium of magnesium reducing furnace slag production sulphur silicon fertilizer, it is characterized in that: may further comprise the steps:
With the magnesium reducing furnace slag through pulverizer grinding to 100～200 orders;
After magnesium reducing furnace slag behind the grinding and Hydrogen chloride fully react, filter out filter residue, promptly silica polymer is subsequent use with the silica polymer oven dry grinding that obtains; Said Hydrogen chloride concentration is between 15～25%;
Filtrating is divided into two parts of A, B; A, B ratio are 1: (1.7～2); After A solution and dilute sulphuric acid fully reacted, evaporative crystallization went out the mixed crystal of calcium sulfate and sal epsom, and B solution goes out to contain the mixed crystal of calcium chloride and magnesium chloride 100～150 ℃ of following direct evaporation crystallizations; Said dilute sulphuric acid concentration is between 25～40%;
The mixed crystal of silica polymer, calcium chloride crystal and magnesium chloride, calcium sulfate and sal epsom mixed crystal are mixed the back granulation, get final product calcium magnesium sulphur silicon fertilizer.
2. the technology of utilizing the efficient calcium magnesium of magnesium reducing furnace slag production sulphur silicon fertilizer according to claim 1, it is characterized in that: the composition of the magnesium reducing furnace slag in the said step (1) is: CaO:45～58%, MgO:7～10%, SiO
2: 25～35%, Fe
2O
3: 4～5%, Al
2O
3Ignore.
3. the technology of utilizing the efficient calcium magnesium of magnesium reducing furnace slag production sulphur silicon fertilizer according to claim 1 and 2 is characterized in that: the proportional range of the required magnesium reducing furnace slag of the said technology of utilizing the efficient calcium magnesium of magnesium reducing furnace slag production sulphur silicon fertilizer, Hydrogen chloride, dilute sulphuric acid is 1: (2～2.5): (1.5～2).
4. the technology of utilizing the efficient calcium magnesium of magnesium reducing furnace slag production sulphur silicon fertilizer according to claim 1 is characterized in that: after will drying in the said step (2) silica polymer grinding to 100～200 orders.
5. the technology of utilizing the efficient calcium magnesium of magnesium reducing furnace slag production sulphur silicon fertilizer according to claim 1 is characterized in that: be to utilize vacuum filtration to leach filter residue in the said step (2).
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| CN2010105537039A CN102030566B (en) | 2010-11-22 | 2010-11-22 | New process for producing efficient calcium magnesium sulphur silicon fertilizer by utilizing slag from magnesium reduction furnace |
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| CN2010105537039A CN102030566B (en) | 2010-11-22 | 2010-11-22 | New process for producing efficient calcium magnesium sulphur silicon fertilizer by utilizing slag from magnesium reduction furnace |
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| CN102030566A CN102030566A (en) | 2011-04-27 |
| CN102030566B true CN102030566B (en) | 2012-08-22 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102807457B (en) * | 2012-09-01 | 2014-06-25 | 曹志强 | Mineral nutrient for ginseng and American ginseng and preparation method of mineral nutrient |
| CN103553109B (en) * | 2013-10-11 | 2015-07-01 | 银川能源学院 | Comprehensive utilization method of magnesium-smelting slag from Pidgeon process |
| CN104649784B (en) * | 2015-02-09 | 2017-06-23 | 山西大学 | A kind of method that Si-K fertilizer is prepared based on magnesium slag |
| CN104628479A (en) * | 2015-02-09 | 2015-05-20 | 山西大学 | Method for preparing controlled release compound fertilizer through magnesium slag phosphorus acid passivation |
| CN106180121B (en) * | 2016-07-06 | 2018-09-04 | 洪昆喨 | A kind of processing method of converter stone waste material |
| CN106187330A (en) * | 2016-07-08 | 2016-12-07 | 贵州鑫亚矿业有限公司 | A kind of amorphous silica prepares the method for high-quality solubility in citric acid siliceous fertilizer |
| CN110734349B (en) * | 2019-10-31 | 2022-06-07 | 西安交通大学 | Calcium-magnesium-phosphorus compound fertilizer prepared from waste residues generated in magnesium smelting by Pidgeon process and method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1102172A (en) * | 1993-10-28 | 1995-05-03 | 太原钢铁公司 | Multielement compound fertilizer and making method thereof |
| JP2000034185A (en) * | 1998-07-21 | 2000-02-02 | Denki Kagaku Kogyo Kk | Inorganic composition, its production, fertilizer and soil conditioner using the same |
| CN1923764A (en) * | 2006-03-15 | 2007-03-07 | 岳玉友 | Silicon, calcium and magnesium fertilizer |
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2010
- 2010-11-22 CN CN2010105537039A patent/CN102030566B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1102172A (en) * | 1993-10-28 | 1995-05-03 | 太原钢铁公司 | Multielement compound fertilizer and making method thereof |
| JP2000034185A (en) * | 1998-07-21 | 2000-02-02 | Denki Kagaku Kogyo Kk | Inorganic composition, its production, fertilizer and soil conditioner using the same |
| CN1923764A (en) * | 2006-03-15 | 2007-03-07 | 岳玉友 | Silicon, calcium and magnesium fertilizer |
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