CN101857467B - Process method for preparing potassium fertilizer by reaction of ammonia evaporation wastewater in soda plant and potash feldspar - Google Patents
Process method for preparing potassium fertilizer by reaction of ammonia evaporation wastewater in soda plant and potash feldspar Download PDFInfo
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- CN101857467B CN101857467B CN2010101778661A CN201010177866A CN101857467B CN 101857467 B CN101857467 B CN 101857467B CN 2010101778661 A CN2010101778661 A CN 2010101778661A CN 201010177866 A CN201010177866 A CN 201010177866A CN 101857467 B CN101857467 B CN 101857467B
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- ammonia liquid
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Abstract
The invention provides a process method for preparing a potassic fertilizer by reaction of ammonia evaporation wastewater in a soda plant and potash feldspar, which comprises the following steps of: (1) taking ammonia evaporation waste liquor; (2) uniformly mixing the ammonia evaporation waste liquor and potash feldspar powder in a weight ratio of the total weight of CaCl2 and NaCl contained in the ammonia evaporation waste liquor to the weight of the potash feldspar powder of 0.05-0.2:1; and (3) roasting at the temperature of between 700 and 1,300 DEG C for 2 to 4 hours. The ammonia evaporation waste liquor is taken as a raw material and is changed into treasure, so the long-term influence of a large amount of ammonia evaporation waste liquor in the soda plant on the environment is radically eliminated, the whole production process has no secondary pollution, and the process method has good social benefit. In addition, the ammonia evaporation waste liquor is directly and effectively utilized to prepare water-soluble potassic fertilizers and KCl crystal materials, and has wide application range and obvious economic benefit. The process method has the advantages of simple process, low production cost and suitability for promotion and application.
Description
Technical field
The present invention relates to method, relate in particular to a kind of method of producing potash fertilizer with soda factory evaporated waste ammonia liquid and potassium felspar sand reaction the trade effluent utilization of waste material.
Background technology
In the production of Sol dimension method soda ash, generally include following steps: ammoniated brine carbonating, the heavy alkali of separation and recovery ammonia, wherein reclaim ammonia and be meant that in ammonia steaming system, adding milk of lime also uses the vapor distillation ammonia.Behind aforesaid operations, contain 2～3% solid matter in the gained liquid, this liquid is " alkaline residue " through solid-liquid separation gained solid, and its staple is CaCO
3, CaCl
2, CaO and Mg (OH)
2Deng, gained liquid is " evaporated waste ammonia liquid ", its staple is CaCl
2And NaCl.Usually, one ton of soda ash of every production produces 0.2～0.3 ton of alkaline residue and 10～12 tons of evaporated waste ammonia liquids approximately.The growing amount of evaporated waste ammonia liquid is 30～50 times of alkaline residue growing amount.
For a long time, the processing for evaporated waste ammonia liquid never has ideal method with utilization.The soda factory evaporated waste ammonia liquid is directly entered environment, environment is caused seriously influence.Once there was factory that evaporated waste ammonia liquid is carried out reclaiming CaCl after the evaporation concentration
2And NaCl, but because of waste strength is rare, need to consume great amount of heat energy, and wastewater flow rate is big, and CaCl
2Purposes limited, market capacity is less, thereby fails industrializing implementation.
Patent of invention CN1298848A provides a kind of process method of utilizing soda factory alkaline residue, waste liquid and potassium ore as raw material system potash fertilizer.This method utilizes alkaline residue, mother liquor of calcium and potassium felspar sand to produce solubility potash fertilizer as raw material, and wherein evaporated waste ammonia liquid is as preparing burden in the grog after the ratio adding roasting of liquid-solid ratio 1: 0.8～1.This ratio is very little for the growing amount of annual evaporated waste ammonia liquid is about 30～50 times of alkaline residue growing amount, so this method is enough to solve the problem that a large amount of evaporated waste ammonia liquids of soda factory need be handled far from.
Secondly, evaporated waste ammonia liquid has neither part nor lot in the reaction that solubility potash fertilizer is extracted in high-temperature roasting, i.e. CaCl in the evaporated waste ammonia liquid
2Be not used effectively in preparation potash fertilizer with the NaCl composition.This method fails to effectively utilize evaporated waste ammonia liquid.
In addition, this method needs with a large amount of mother liquor of calcium as reaction raw materials, promptly before the reaction beginning as if unripe this mother liquor of calcium, this method then can not be suitable for.
To sum up, the process method that patent of invention CN1298848A provides is inappropriate for direct processing and utilizes a large amount of soda ash evaporated waste ammonia liquids, has certain limitation.
Summary of the invention
Technical problem to be solved by this invention is the deficiency to prior art; Proposing a kind of evaporated waste ammonia liquid with the soda factory discharging is raw material; The method of can be in large quantities and directly effectively evaporated waste ammonia liquid being turned waste into wealth is thoroughly eliminated the influence of a large amount of for a long time evaporated waste ammonia liquids to environment.
One aspect of the present invention provides a kind of and has reacted the method for producing potash fertilizer with soda factory evaporated waste ammonia liquid and potassium felspar sand, may further comprise the steps:
(1) gets evaporated waste ammonia liquid;
(2) press CaCl contained in the evaporated waste ammonia liquid
2With the gross weight of NaCl and the weight ratio of potassium felspar sand powder be 0.05～0.2: 1 mixes; And
(3) be 700～1300 ℃ of roastings 2～4 hours in temperature.
" evaporated waste ammonia liquid " is meant the waste water of ammoniated brine after ammonia is reclaimed in carbonating, the heavy alkali of separation and evaporation of Sol dimension method soda factory, staple CaCl
2Be respectively 90～120g/L and 40～60g/L with the content of NaCl.
The present invention be utilize in the evaporated waste ammonia liquid sodium with (or) calcium component can at high temperature react with potassium felspar sand, makes that water-insoluble potassium is converted into water-soluble potassium in the potassium felspar sand, reaction formula is respectively:
KAlSi
3O
8+NaCl＝KCl+NaAlSi
3O
8
2KAlSi
3O
8+CaCl
2＝2KCl+CaAl
2Si
2O
8+4SiO
2。
Evaporated waste ammonia liquid can directly get into step (2) to be mixed with the potassium felspar sand powder, mixes with the potassium felspar sand powder after also can and reclaiming the NaCl crystal through evaporation concentration.Preferably, the evaporated waste ammonia liquid of step (1) can be the waste water of isolating after the further evaporation concentration behind the NaCl crystal.Step (1) can comprise with evaporated waste ammonia liquid evaporation concentration to solids content be 40～45% the back and isolate the NaCl crystal, get waste water.Isolated NaCl crystal can be used for industrial salt, still contains CaCl in the remaining waste water
2With part NaCl composition.
The middle potassium felspar sand powder of step (2) is crossed 100～200 mesh sieves and is prepared after grinding, preferably, the potassium felspar sand powder is crossed 100 mesh sieves.
In the step (2) evaporated waste ammonia liquid or the waste water after separating the NaCl crystal are pressed CaCl contained in the waste water
2With the gross weight of NaCl and the weight ratio of potassium felspar sand powder be 0.05～0.2: 1 mixes.Preferably, contained CaCl in step (2) evaporated waste ammonia liquid
2With the gross weight of NaCl and the weight ratio of potassium felspar sand powder be 0.10～0.15: 1.
Compound in the step (2) can directly get into step (3), also can be made into to get into step (3) behind the agglomerate.Preferably, step (2) further comprises in mixed evaporated waste ammonia liquid and potassium felspar sand powder and to add that to account for potassium felspar sand powder weight be 6～8% fuel, processes agglomerate after mixing with evaporated waste ammonia liquid and potassium felspar sand.
Equally preferably, can be earlier evaporated waste ammonia liquid evaporation concentration to solids content 40～45%, get the waste water that separates behind the NaCl crystal then, add the potassium felspar sand powder, process agglomerate after mixing.More preferably, step (2) further comprises in waste water and the potassium felspar sand powder after separating the NaCl crystal and adds fuel, processes agglomerate after mixing, and wherein, weight of fuel is 6～8% of a potassium felspar sand powder weight.
The purpose that adds fuel is in order to make compound reach needed high temperature.In order to reach a high temperature, can adopt external-heat, also can adopt with coal or oil or combustible gas is the internal heat type of fuel, wherein, is that fuel cost is minimum with the coal.Therefore, preferably, fuel is coal-fired powder.
The method of processing agglomerate can be for preparing with agglomerating equipment such as disk balling machine or single-lead-screw extruding briquetting machine.
Step (3) for the compound in the step (2) or the agglomerate of processing after mixing drop in the roasting kiln, at the kiln discharge after 2～4 hours of roasting under 700～1300 ℃ the high temperature, for burning till material.
Used roasting apparatus can be that shaft kiln also can be the kiln of rotary kiln or other type.
With NaCl or (with) CaCl
2The reaction of method and potassium felspar sand belongs to the infiltration method, only make NaCl or (with) CaCl
2Fusing can make just that the potassium better conversion is a water-soluble potassium in the potassium felspar sand.Preferably, temperature is controlled to be 800～1000 ℃.More preferably, temperature is controlled to be 900～1000 ℃.
After roasting, the potassium in the potassium felspar sand powder has 70～90% to be converted into water-soluble potassium, burns till soluble potassium content in the material (with K
2The O meter) reaches more than 7%.Burn till material and can directly be used as potash fertilizer, or be used for the fertile raw material of compound, also can pass through processes such as lixiviate, evaporation concentration, crystallization, process purified KCl.
Preferably, the present invention can further comprise step (4): burn till the material lixiviate with what obtain after the roasting in the step (3), extracting solvent is 1～3: 1 with the envelope-bulk to weight ratio that burns till material, and extraction time is 1～3 hour, filters, and collects extracting solution and soaks slag.
Wherein, leaching process is the water-soluble potassium that burns till in the material in order to separate.
Extract solvent and do not limit, can be the evaporated waste ammonia liquid that uses in the process of the present invention, also can also be the water equal solvent for the waste water of evaporated waste ammonia liquid after separating the NaCl crystal.Preferably, extraction solvent of the present invention is a water.
This process can adopt still formula equipment to carry out batch operation, or the operate continuously of many stills tandem, or adopts the continuous extraction groove to carry out operate continuously.
Leaching process can carry out at normal temperatures, also can heat, and carries out being no more than under 100 ℃ the temperature.
Carry out liquid-solid separation with filtration unit after the lixiviate, liquid is extracting solution, and solid is the water logging slag.The water logging slag can be used for producing ceramic tile, and extracting solution can further be utilized as industrial raw material.
Preferably, the present invention further comprises step (5): with extracting solution in the step (4) concentrate, crystallization, filtration, separation, obtain the KCl crystallization.
Extracting solution evaporation concentration in vaporizer is approaching saturated to KCl, at this moment there is NaCl to crystallize out, take advantage of heat filtering to isolate NaCl, cooling crystallizes out KCl then, refilters, and obtains the KCl crystallization, with becoming purified KCl product after a small amount of washing.Turn back to recycle in the vaporizer the female night after separating KCl again.When Recycling Mother Solution many times after, CaCl
2When content was higher, not recycling of mother liquor and was used for adding the potassium felspar sand powder after evaporated waste ammonia liquid mixes.Add-on may command KCl crystalline quality through control waste water.
The present invention provides a kind of application of method in producing potash fertilizer and purified KCl of producing potash fertilizer with soda factory evaporated waste ammonia liquid and potassium felspar sand reaction on the other hand.
Compared with prior art, the present invention has following advantage:
(1) the present invention adopts evaporated waste ammonia liquid as raw material, and a large amount of evaporated waste ammonia liquids is turned waste into wealth, and has thoroughly eliminated the influence that soda factory a large amount of evaporated waste ammonia liquids for a long time cause environment, and the whole process of production non-secondary pollution produces, and has good social benefit;
(2) the present invention directly effectively utilizes evaporated waste ammonia liquid and makes raw materials such as water soluble potassic fertilizer, KCl crystal and water logging slag, and its purposes is wide, has remarkable economic efficiency; And
(3) technology of the present invention is simple, the required cost of production is low, is fit to apply.
Description of drawings
Fig. 1 is a method flow synoptic diagram of the present invention.
Embodiment
The following stated is a preferred implementation of the present invention; Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention; Can also make some improvement and retouching, these improvement and retouching also are regarded as protection scope of the present invention.
Embodiment one
React the process method of producing potash fertilizer with soda factory distilled ammonia wastewater and potassium felspar sand, may further comprise the steps:
(1) gets evaporated waste ammonia liquid, its staple CaCl
2Be respectively 100g/L and 50g/L with the content of NaCl.
(2) mixed by every liter of evaporated waste ammonia liquid and 1.5kg potassium felspar sand powder is even.
(3) add roasting in the rotary kiln, the roast area temperature is 700 ℃, discharges at the bottom of kiln through burning till material after 4 hours.Burn till soluble potassium content in the material (with K this moment
2The O meter) be 7%.This burns till material can directly be used as potash fertilizer.
Embodiment two
React the process method of producing potash fertilizer with soda factory distilled ammonia wastewater and potassium felspar sand, may further comprise the steps:
(1) gets evaporated waste ammonia liquid, its staple CaCl
2Be respectively 110g/L and 40g/L with the content of NaCl.
(2) mixed by every liter of evaporated waste ammonia liquid and 0.75kg potassium felspar sand powder is even.
(3) add roasting in the rotary kiln, the roast area temperature is 1200 ℃, discharges at the bottom of kiln through burning till material after 2 hours.Burn till soluble potassium content in the material (with K this moment
2The O meter) be 8%.This burns till material can directly be used as potash fertilizer.
Embodiment three
Shown in accompanying drawing 1, react the process method of producing potash fertilizer with soda factory distilled ammonia wastewater and potassium felspar sand, may further comprise the steps:
(1) get evaporated waste ammonia liquid, evaporation concentration to solids content is 40～45%, and the NaCl that fractional crystallization comes out gets waste water.
(2) press feldspar in powder: evaporated waste ammonia liquid solids content (contained CaCl
2And NaCl): the weight ratio of coal dust is that 100: 15: 6 ratio adds in the mixing machine and mixes, and going into to process in the disk balling machine diameter then is the ball about 15mm.
(3) add roasting in the shaft kiln, the roast area temperature is 1000 ℃, discharges at the bottom of kiln through burning till material after 2 hours.
(4) will burn till material through pulverizing and crossing 100 mesh sieves, and add in the entry in 1: 1 ratio, through the two-stage countercurrent lixiviate, about 1 hour of extraction times at different levels are isolated water logging slag and extracting solution then.Can be fired into ceramic tile behind the clay of water logging slag adding 15%.
(5) extracting solution is closely saturated to KCl through three-effect evaporation and condensation, heat filtering then, and crystallisation by cooling obtains solid K Cl after the separation again, and purity can reach more than 96%.
Embodiment four
React the process method of producing potash fertilizer with soda factory distilled ammonia wastewater and potassium felspar sand, may further comprise the steps:
(1) get evaporated waste ammonia liquid, evaporation concentration to solids content 40～45%, the NaCl that fractional crystallization comes out gets waste water.
(2) press feldspar in powder (crossing 100 mesh sieves): evaporated waste ammonia liquid solids content (contained CaCl
2And NaCl): the weight ratio of coal dust is that 100: 15: 7 ratio adds in the mixing machine and mixes.
(3) add roasting in the shaft kiln, the roast area temperature is 900 ℃, discharges at the bottom of kiln through burning till material after 3 hours.
(4) will burn till material through pulverizing and crossing 100 mesh sieves, add in the entry,, isolate water logging slag and extracting solution then through 2 hours lixiviate in 1: 2 ratio.Can be fired into ceramic tile behind the clay of water logging slag adding 15%.
(5) extracting solution is closely saturated to KCl through three-effect evaporation and condensation, heat filtering then, and crystallisation by cooling obtains solid K Cl after the separation again, and purity can reach more than 96%.
Claims (10)
1. produce the process method of potash fertilizer with soda factory distilled ammonia wastewater and potassium felspar sand reaction, it is characterized in that, may further comprise the steps:
(1) gets evaporated waste ammonia liquid;
(2) by contained CaCl in the said evaporated waste ammonia liquid
2With the gross weight of NaCl and the weight ratio of potassium felspar sand powder be 0.05～0.2: 1 mixes; And
(3) be 700～1300 ℃ of roastings 2～4 hours in temperature.
2. the method for claim 1 is characterized in that, the evaporated waste ammonia liquid of said step (1) is the waste water of isolating after the further evaporation concentration behind the NaCl crystal.
3. the method for claim 1 is characterized in that, contained CaCl in said step (2) evaporated waste ammonia liquid
2With the gross weight of NaCl and the weight ratio of potassium felspar sand powder be 0.10～0.15: 1.
4. the method for claim 1 is characterized in that, said step (2) further comprises in the mixture of evaporated waste ammonia liquid and potassium felspar sand powder and to add that to account for potassium felspar sand powder weight be 6～8% fuel, processes agglomerate after mixing.
5. method as claimed in claim 4 is characterized in that, said fuel is coal-fired powder.
6. the method for claim 1 is characterized in that, temperature is 800～1000 ℃ in the said step (3).
7. the method for claim 1 is characterized in that, further comprises burning till the material lixiviate with what obtain after the roasting in the said step (3); Extracting solvent is 1～3: 1 with the envelope-bulk to weight ratio that burns till material; Extraction time is 1～3 hour, filters, and collects extracting solution and soaks slag.
8. method as claimed in claim 7 is characterized in that, said extraction solvent is a water.
9. method as claimed in claim 7 is characterized in that, further comprise with extracting solution concentrate, crystallization, filtration, separation, obtain the KCl crystallization.
10. the described method of the arbitrary claim of claim 1-9 is used to produce potash fertilizer and KCl.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101778661A CN101857467B (en) | 2010-05-20 | 2010-05-20 | Process method for preparing potassium fertilizer by reaction of ammonia evaporation wastewater in soda plant and potash feldspar |
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|---|---|---|---|
| CN2010101778661A CN101857467B (en) | 2010-05-20 | 2010-05-20 | Process method for preparing potassium fertilizer by reaction of ammonia evaporation wastewater in soda plant and potash feldspar |
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| CN103664242B (en) * | 2013-09-18 | 2015-07-22 | 薛彦辉 | Caustic sludge treatment method |
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