CN101428769A - Method for production of kalium-calcium fertilizer and joint production of sulphuric acid with insoluble kalium-containing rock and phosphogypsum - Google Patents
Method for production of kalium-calcium fertilizer and joint production of sulphuric acid with insoluble kalium-containing rock and phosphogypsum Download PDFInfo
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- CN101428769A CN101428769A CNA200810069029XA CN200810069029A CN101428769A CN 101428769 A CN101428769 A CN 101428769A CN A200810069029X A CNA200810069029X A CN A200810069029XA CN 200810069029 A CN200810069029 A CN 200810069029A CN 101428769 A CN101428769 A CN 101428769A
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- phosphogypsum
- potash
- sulfuric acid
- bearing rock
- insoluble potassium
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Abstract
The invention relates to a method for producing potassium-calcium fertilizer co-production sulphuric acid by using insoluble potassium-bearing rocks and phosphogypsum, and belongs to the technical field of the disposal of three wastes and the chemical production. The method comprises the following steps: the insoluble potassium-bearing rocks, the phosphogypsum and anthracitic coal are mixed at the mass ratio of 1:0.7-2.2:0.05-0.25; the obtained mixture is reductively calcined in a rotary kiln, a vertical kiln or a tunnel kiln at 1000 to 1200 DEG C for 20 to 150 minutes after grinding, ball production or block production; clinker aggregate is sintered to be in a shattered state and packed into potassium-calcium fertilizer products; and tail gas is delivered to a sulphuric acid preparation system to prepare the sulphuric acid. One of main raw materials for producing potassium-calcium fertilizers is industrial residues. Therefore, compared with a method for producing the sulphuric acid by using the phosphogypsum, the invention has more advantages.
Description
Technical field: the present invention relates to the method that insoluble potassium bearing rock of a kind of usefulness and phosphogypsum are produced silico-calcium potash fertilizer (or claiming potash-lime fertilizer) co-producing sulfuric acid, belong to enviromental protection and improvement and chemical production technical field.
Background technology: though that China can be directly used in the water-soluble potassium ore resources of producing potash fertilizer is few, insoluble potassium ore resources is very abundant.Potassium felspar sand is exactly wherein more important a kind of.Potassium felspar sand had not only contained potassium but also siliceous, and chemical formula is K
2OAl
2O
36SiO
2, contain K
2O16.9%, Al
2O
318.4%, SiO
264.7%.Although the content of potassium oxide is not very too high in the potassium felspar sand, its reserves in the earth's crust is big, and it is wide to distribute.These potassium ore resources if can be used to produce potash fertilizer, just overcome China's potash fertilizer resources of production problem of shortage, but mass production potash fertilizer produces significant role to promoting China's agricultural development.To being that the potassium ore resources of representative is that the method for raw material production potash fertilizer mainly contains following two classes with the potassium felspar sand:
(1) high-temperature roasting class.Potassium felspar sand, Wingdale and coal (as fuel) are ground into powder by a certain percentage, add the laggard capable high-temperature roasting of less water mixing balling-up, utilize calcium oxide to destroy the structure of potassium felspar sand mineral, pulverize again, be potash-lime fertilizer.At present, the method transformation efficiency that potash-lime fertilizer is produced in high-temperature roasting is the highest, and that quality product is best is patent " a kind of production method of potash-lime fertilizer " the application number 92111690.X of Guizhou University, adopts clamp dog flint road klining knot.Its clamp dog agglomerating principle has points of resemblance with the present invention.(2) wet extraction class.Under certain temperature and pressure, ore is handled, made the potassium in the ore change soluble substance into, make it leach out then, make potash fertilizer such as the higher Repone K of purity, vitriolate of tartar with acid, alkali or salt etc.Wet extraction prepares that problem that potash fertilizer exists is that flow process complexity, energy consumption are higher, the silicon components in the potassium ore deposit is not rationally utilized, extracts the back and produces shortcomings such as a large amount of waste residues, is difficult to industrializing implementation.
The residue phosphogypsum major ingredient of Wet-process Phosphoric Acid Production is CaSO
42H
2O, at present main processing mode is stacked for the slag field, and mostly pile up like a mountain, becomes public hazards.It is a great problem that the phosphate production industry is badly in need of solution.Some enterprise is used to produce cement by-product sulfuric acid, and domestic Shandong northern Shandong chemical industry and Sichuan Yin Shan chemical industry have all been realized industrialization, and its technological process of production is: phosphogypsum reduces free P in the phosphogypsum through washing, purifying
2O
5Content with F makes P
2O
5Content less than 1%, F content is less than 0.35%, enters water extracter and dryer then, the phosphogypsum that has removed part moisture and part fluorine enters batch bin after cooling.Hard coal, silica and various auxiliary material enter batch bin after reaching granularity requirements through ball mill grinding, and the cement slurry for preparing enters calcined by rotary kiln through after the homogenizing, and it is that reductive agent resolves into CaO and SO with carbon for about 1300 ℃ that phosphogypsum decomposes section at rotary kiln
2, CaO further generates Dicalcium Phosphate (Feed Grade) (C with the reaction of silica generation mineralising for about 1450 ℃ in the rotary kiln section of burning till
2S) and tricalcium silicate (C
3S) finish the reaction of burning till cement, the material that goes out rotary kiln is cement clinker, behind raw materials such as cooling adding part retardant and activator, obtains cement products through grinding.Contain SO
2Kiln gas be and produce the vitriolic unstripped gas, unstripped gas is through dedusting, purification, unstripped gas is through purifying SO
2Back concentration dilution is a concentration expressed in percentage by volume about 4%, for the thermal equilibrium that guarantees to transform, adopts one to change one and inhale the relieving haperacidity flow process usually, total turnover ratio about 96%, emptying tail gas SO
2Concentration have only could qualified discharge through vent gas treatment.The flow process of the phosphogypsum system producing sulfuric acid and jointly cement of domestic industryization has following shortcoming: unstripped gas SO at present
2Concentration low, double conversion and double absorption transforms heat can not balance, can only change a suction with one, directly emptying of tail gas, running expense is higher.Concentration is low to cause the production unit production intensity low, causes the sulphuric acid plant investment bigger, and usefulness is low.The foreign matter content of raw material phosphogypsum such as fluorine, phosphorus are required content＜1%, and phosphogypsum need just can be used for producing through pre-treatment.Kiln operational requirement complexity causes the cement product quality instability simultaneously.
Still there be not at present any patent application and correlation technique of producing the potash-lime fertilizer co-producing sulfuric acid with phosphogypsum, than producing cement joint production sulfuric acid more superiority is arranged and produce the potash-lime fertilizer co-producing sulfuric acid with phosphogypsum with phosphogypsum, comprise that technology is simple, processing ease, constant product quality, cut down the consumption of energy greatly, open up a new way for solving the phosphogypsum three-waste pollution.
Summary of the invention: purpose of the present invention, be to open up a new approach, effectively utilize the calcium oxide in the phosphogypsum to produce potash-lime fertilizer, reduce the potash-lime fertilizer production cost greatly for phosphogypsum slag effectively utilizes, effectively utilize the S in the phosphogypsum to produce sulfuric acid, phosphogypsum is turned waste into wealth.
The present invention is achieved like this: is that 1:0.7～2.2:0.05～0.25 proportioning is mixed with insoluble potassium bearing rock, phosphogypsum and hard coal by mass ratio, grinding to 80～120 orders, after making φ 10～30mm bead or corresponding piece at rotary kiln, interior 1000～1200 ℃ of roastings of shaft kiln or tunnel furnace 20～150 minutes, sintered clinker is through fragmentation, packing is potash fertilizer products behind the grinding, and tail gas send the sulfuric acid preparation system.In the batching, phosphogypsum is with CaSO
4Content meter, coal are in the fixed carbon amount.
The insoluble potassium bearing rock of indication of the present invention be meant with the potassium felspar sand be representative contain potassium silicate class potassium ore resources.
Insoluble potassium bearing rock of a kind of usefulness of indication of the present invention and phosphogypsum are produced the method for potash-lime fertilizer co-producing sulfuric acid, the gypsum that other sulfur acid calcium such as the same suitable plaster of paris, desulfurated plaster, fluorgypsum are main component except that phosphogypsum.
Insoluble potassium bearing rock of the present invention and phosphogypsum, anthracitic optimum ratio are 1:1.8～2:0.1～0.12 by mass ratio, and phosphogypsum is not to contain the CaSO of crystal water in the proportioning
4Meter is heavy, and hard coal in fixed carbon heavily.
Insoluble potassium bearing rock of the present invention and phosphogypsum, hard coal mix back grinding to 80～120 order preferable range, 100～120 orders.
Insoluble potassium bearing rock behind the grinding of the present invention and phosphogypsum, hard coal powder add water and make coccoid or blocky material piece.
The reducing roasting of the present invention in kiln is meant that temperature is 1000～1200 ℃, and roasting time is 20～90 minutes, is preferably 1100～1050 ℃ of roastings 40～60 minutes, O in the control kiln exhaust gas
2Concentration expressed in percentage by volume 0.5～1.0%.
Sintered clinker of the present invention fineness behind broken, grinding reaches 80～100 orders (tail over＜5%), through being packaged into the potash-lime fertilizer product.
SO in the kiln exhaust gas of the present invention
2Concentration expressed in percentage by volume is 5～8%.SO
2Behind dust cleaning, send the sulphur preparation to be equipped with system with the tail gas discharge, under the effect of catalyzer, change into SO as unstripped gas
3, SO
3After inhaling, water gets sulfuric acid.
The present invention has following feature and beneficial effect:
Containing the potassium main component in the insoluble potassium bearing rock is potassium felspar sand (K
2OAl
2O
36SiO
2), at high temperature with the phosphogypsum reduction decomposition after CaO reaction, make the insoluble K in the potassium ore
2O changes processable and solubility in citric acid K into
2O can be absorbed by crop.Its principal reaction is as follows:
2CaSO
4+C→2CaO+2SO
2+CO
2
K
2O·Al
2O
3·6SiO
2+6CaO→K
2O·Al
2O
3+6(CaO·SiO
2)
The present invention compares with the existing method of utilizing insoluble potassium bearing rock to produce potash fertilizer, have following beneficial effect: (1) existing high-temperature roasting prepares in the potash fertilizer technology, the raw material that reacts with potassium felspar sand is the ore that Wingdale, rhombspar etc. contain CaO, the present invention's industrial residue phosphogypsum, be utilization of waste material, also make contributions for environmental protection.(2) raw material of the present invention and potassium felspar sand pyroreaction is a phosphogypsum, contains impurity such as fluoride salt, ferric oxide in the phosphogypsum, has reduced the fusing point of material, and sintering just can realize that 1000～1200 ℃ of temperature prior art generally will be more than 1200 ℃.(3) the present invention's by-product when high temperature sintering goes out potash-lime fertilizer goes out to produce vitriolic SO
2Gas has improved economic benefit.
The present invention compares with existing technology with phosphogypsum system sulfuric acid by-product cement, has following beneficial effect: SO in (1) kiln exhaust gas of the present invention
2The concentration height.In the existing phosphogypsum process for preparing sulfuric acid, the CaSO in the phosphogypsum
4Reduction decomposition in kiln is reacted based on following reaction:
2C+O
2→2CO
CaSO
4+CO→CaO+SO
2+CO
2
Finish mix or pellet after the present invention adopts potassium ore deposit, phosphogypsum, hard coal is levigate, the CaSO in the phosphogypsum
4Reduction decomposition in kiln is reacted based on following reaction:
2CaSO
4+C→2CaO+2SO
2+CO
2
By above-mentioned reaction as can be known, 1 mole of SO of every generation in the existing phosphogypsum process for preparing sulfuric acid
2, will 1 mole of CO of association
2, 1 mole of SO of the every generation of the present invention
2, 0.5 mole of CO of an association
2, waste gas CO in the kiln exhaust gas
2Volumetric concentration reduces, SO
2Volumetric concentration increases.(2) maturing temperature of the present invention is low.In the existing phosphogypsum relieving haperacidity jointly producing cement technology, in order to reach cement clinker quality, maturing temperature is more than 1350 ℃.Maturing temperature of the present invention just can be finished below 1200 ℃.(3) phosphogypsum of the present invention does not need to carry out defluorinate, dephosphorization pre-treatment.In the existing phosphogypsum relieving haperacidity jointly producing cement technology,, require P in the phosphogypsum owing to will take into account cement quality
2O
5Content less than 1%, F content is less than 0.35%, this index is to be beyond one's reach without pretreated phosphogypsum.The present invention does not require These parameters because grog is a fertilizer product.(4) clinker quality of the present invention is easy to control.In the existing phosphogypsum relieving haperacidity jointly producing cement technology, sintered clinker is a cement clinker, and its quality is subjected to CaSO in proportioning raw materials, phosphogypsum foreign matter content, the phosphogypsum
4Influence such as reduction decomposition degree is very big, and the cement quality fluctuation is big.Proportioning of the present invention is loose relatively, and the phosphogypsum foreign matter content is not had particular requirement, CaSO in the phosphogypsum
4Reduction decomposition degree etc. are to clinker quality (effective K
2O) influence is less, and clinker quality is easy to control.
Embodiment: embodiment 1:
Raw material 1: potassium felspar sand, collecting location: Feng County, Jiangsu
The chemical constitution of potassium felspar sand sees the following form
Raw material 2: phosphogypsum, collecting location: Guizhou Xiyang Fertilizer Industry Co., Ltd.
The phosphogypsum chemical constitution sees the following form
Raw material 3: hard coal (place of production: Guizhou Jinsha, fixed carbon content 85.2%)
Implementation method:
Is that 1:0.1:1.8 prepares burden with electronic scales with the potassium felspar sand after the preliminary fragmentation, hard coal and phosphogypsum by mass ratio, and phosphogypsum is with CaSO in the batching
4Meter is heavy, and hard coal in fixed carbon heavily.Mixture drying machine oven dry back is with ball mill grinding to 120 order (tail over＜5%), powder adds the water balling-up in dribbling balling machine, spherolite directly is controlled at φ 10～φ 30mm, moisture 10%～15%, pellet is sent reducing roasting in the rotary kiln back to after preliminary oven dry, 1100 ℃ of roasting time of control high temperature 40 minutes, O in the kiln exhaust gas
2Volumetric concentration 0.8%, kiln exhaust gas are sent sulfuric acid preparation system system sulfuric acid through dedusting, after purifying, and sintered clinker with ball mill grinding to 80 order, tails over after cooling off＜5% be the potash-lime fertilizer finished product after packing.
Result of implementation:
1. fertilizer prepares part
Zhi Bei potash-lime fertilizer effective constituent sees the following form after testing
As seen from the above table, each the effective constituent index of potash-lime fertilizer by the industrial test preparation meets company standard.K in the potassium ore
2The O transformation efficiency reaches 98%, simultaneously SiO
2, CaO, MgO all become can be by the effective constituent of crop absorption, the effective constituent total content reaches 72.4%.
2. sulfuric acid prepares part
SO in the kiln exhaust gas after testing
2Volumetric concentration 8%, CaSO in the phosphogypsum
4The reduction decomposition rate reaches 95%.
Embodiment 2:
Raw material 1: potassium felspar sand, collecting location: Guizhou Fuquan
The chemical constitution of potassium felspar sand sees the following form
Raw material 2: phosphogypsum, collecting location: Guizhou Xiyang Fertilizer Industry Co., Ltd.
The phosphogypsum chemical constitution sees the following form
Raw material 3: hard coal, the place of production: Guizhou Jinsha, fixed carbon content 85.2%
Implementation method:
Is that 1:0.12:2.0 prepares burden with electronic scales with the potassium felspar sand after the preliminary fragmentation, hard coal and phosphogypsum by mass ratio, phosphogypsum CaSO in the batching
4Meter is heavy, coal in fixed carbon heavily, mixture drying machine oven dry back (tails over＜5%=with ball mill grinding to 120 order, powder adds the water balling-up in dribbling balling machine, spherolite directly is controlled at φ 10～φ 30mm, and is moisture 10%～15%, and pellet is sent reducing roasting in the rotary kiln back to after preliminary oven dry, 1050 ℃ of roasting time of control high temperature 60 minutes, O in the kiln exhaust gas
2Volumetric concentration 0.8%, kiln exhaust gas are sent sulfuric acid preparation system system sulfuric acid through dedusting, after purifying, and sintered clinker with ball mill grinding to 80 order, tails over after cooling off＜and 5%, be silico-calcium potash fertilizer (or title potash-lime fertilizer) finished product after the packing.
Result of implementation:
1. fertilizer prepares part
Zhi Bei potash-lime fertilizer effective constituent sees the following form after testing
As seen from the above table, each the effective constituent index of silico-calcium potash fertilizer by the industrial test preparation meets company standard.K in the potassium ore
2The O transformation efficiency reaches 97%, simultaneously SiO
2, CaO, MgO all become can be by the effective constituent of crop absorption, the effective constituent total content reaches 72.2%.
2. sulfuric acid prepares part
SO in the kiln exhaust gas after testing
2Volumetric concentration 8%, CaSO in the phosphogypsum
4The reduction decomposition rate reaches 94.5%.
Claims (9)
1. method of producing the potash-lime fertilizer co-producing sulfuric acid with insoluble potassium bearing rock and phosphogypsum, comprise that the sulphur in the phosphogypsum discharges with kiln exhaust gas with the form of sulfurous gas, behind dust cleaning, send the sulfuric acid preparation system to prepare the vitriolic method as unstripped gas, it is characterized in that insoluble potassium bearing rock, phosphogypsum and hard coal are that 1:0.7～2.2:0.05～0.25 proportioning is mixed by mass ratio, grinding to 80～120 orders, after making φ 10～30mm bead or corresponding piece at rotary kiln, interior 1000～1200 ℃ of roastings of shaft kiln or tunnel furnace 20～150 minutes, sintered clinker is through fragmentation, packing is the potash-lime fertilizer product behind the grinding, and tail gas send the sulfuric acid preparation system.
2. the insoluble potassium bearing rock of a kind of usefulness according to claim 1 and phosphogypsum are produced the method for potash-lime fertilizer co-producing sulfuric acid, it is characterized in that insoluble potassium bearing rock be meant with the potassium felspar sand be representative contain potassium silicate class potassium ore resources.
3. according to the method for claim 1 insoluble potassium bearing rock of described a kind of usefulness and phosphogypsum production potash-lime fertilizer co-producing sulfuric acid, it is characterized in that the gypsum that other sulfur acid calcium such as the suitable equally plaster of paris of present method, desulfurated plaster, fluorgypsum are main component.
4. insoluble potassium bearing rock of a kind of usefulness according to claim 1 and phosphogypsum are produced the method for potash-lime fertilizer co-producing sulfuric acid, it is characterized in that insoluble potassium bearing rock and phosphogypsum, anthracitic proportioning are 1:1.8～2.0:0.1～0.12 by mass ratio.
5. insoluble potassium bearing rock of a kind of usefulness according to claim 1 and phosphogypsum are produced the method for potash-lime fertilizer co-producing sulfuric acid, it is characterized in that insoluble potassium bearing rock and phosphogypsum, hard coal mix back grinding preferable range to 100～120 orders, screen over-size＜5%.
6. the insoluble potassium bearing rock of a kind of usefulness according to claim 1 and phosphogypsum are produced the method for potash-lime fertilizer co-producing sulfuric acid, it is characterized in that insoluble potassium bearing rock behind the grinding and phosphogypsum, hard coal powder add water and make coccoid or blocky material piece.
7. insoluble potassium bearing rock of a kind of usefulness according to claim 1 and phosphogypsum are produced the method for potash-lime fertilizer co-producing sulfuric acid, it is characterized in that the reducing roasting in kiln is meant that temperature is 1000～1200 ℃, and roasting time is 20～90 minutes, O in the control kiln exhaust gas
2Concentration expressed in percentage by volume 0.5～1.0%.
8. insoluble potassium bearing rock of a kind of usefulness according to claim 1 and phosphogypsum are produced the method for potash-lime fertilizer co-producing sulfuric acid, it is characterized in that SO in the kiln exhaust gas
2Concentration expressed in percentage by volume is 5～8%.
9. insoluble potassium bearing rock of a kind of usefulness according to claim 1 and phosphogypsum are produced the method for potash-lime fertilizer co-producing sulfuric acid, it is characterized in that sintered clinker fineness behind fragmentation, grinding reaches 80～100 orders, screen over-size＜5%.
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|---|---|---|---|
| CN200810069029XA CN101428769B (en) | 2008-12-09 | 2008-12-09 | Method for production of kalium-calcium fertilizer and joint production of sulphuric acid with insoluble kalium-containing rock and phosphogypsum |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810069029XA CN101428769B (en) | 2008-12-09 | 2008-12-09 | Method for production of kalium-calcium fertilizer and joint production of sulphuric acid with insoluble kalium-containing rock and phosphogypsum |
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| Publication Number | Publication Date |
|---|---|
| CN101428769A true CN101428769A (en) | 2009-05-13 |
| CN101428769B CN101428769B (en) | 2010-11-03 |
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|---|---|---|---|
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| CN108609639A (en) * | 2018-07-03 | 2018-10-02 | 贵州省贵福生态肥业有限公司 | A kind of technique recycling the special potash-lime fertilizer of aluminium coproduction banana using potassium-bearing shale relieving haperacidity |
| CN108715454A (en) * | 2018-07-03 | 2018-10-30 | 贵州省贵福生态肥业有限公司 | The technique of ardealite and the potassium-bearing shale relieving haperacidity recycling special potash-lime fertilizer of aluminium coproduction walnut |
| CN108715455A (en) * | 2018-07-03 | 2018-10-30 | 贵州省贵福生态肥业有限公司 | The technique of ardealite and the potassium-bearing shale relieving haperacidity recycling special potash-lime fertilizer of aluminium coproduction plum |
| CN108928842A (en) * | 2018-07-03 | 2018-12-04 | 贵州省贵福生态肥业有限公司 | The technique of aluminum and coproducing corn fertilizer in a kind of recycling potassium feldspar |
| CN110818470A (en) * | 2019-11-26 | 2020-02-21 | 贵州大学 | Multielement high-efficiency fertilizer for promoting high yield and high quality of plants and fertilizing method |
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