CN105110352A - Method for producing potassium sulfate from potassium/chlorine-ion-containing solid waste - Google Patents
Method for producing potassium sulfate from potassium/chlorine-ion-containing solid waste Download PDFInfo
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Abstract
The invention discloses a method for producing potassium sulfate from potassium/chlorine-ion-containing solid waste, which comprises the following steps: adding water, leaching, adding an alkaline matter and soluble carbonate for impurity removal, and concentrating to obtain a concentrated solution with the K<+> concentration of 100 g/L or above; and adding ammonium sulfate into the concentrated solution, adding a mixture of sodium tripolyphosphate, ammonium monoacid phosphate, magnesium sulfate, urea and sodium salt, reacting to obtain a potassium sulfate precipitate, carrying out solid-liquid separation to obtain wet potassium sulfate and a filtrate, drying to obtain a potassium sulfate product, carrying out concentration and crystallization on the filtrate twice, and drying to obtain a potassium-nitrogen compound fertilizer product. The method is simple and safe, has the advantages of high efficiency, lower cost and high potassium sulfate product quality, does not need any alcohol substance to perform precipitation, and meanwhile, can coproduce the potassium-nitrogen compound fertilizer which satisfies the national standard.
Description
Technical field
The invention belongs to recycling economy field of wastewater reclamation, be specifically related to a kind of method being raw material production potassium sulfate with the solid waste containing potassium, chlorion.
Background technology
The domestic research of the comprehensive utilization technique about sintering dust separation ash and gas ash is started late, and treatment technology also backwardness relatively, still can not meet the requirement of iron and steel solid waste resource high-efficiency recycle.Current most of iron and steel enterprise all adopts mode directly allocated in sintered material by it to fully utilize it.The basic metal in sintering machine head end electro-precipitating dust and beavy metal impurity element are not removed owing to utilizing in process, make impurity element in recycle process by progressively enrichment, and then cause a series of new environmental issue and smelting equipment potential safety hazard accident, these problems constrain again effective utilization of sintering dust separation ash conversely, Some Enterprises is even therefore direct to be abandoned this part sintering ash or landfill disposal, causes the waste of resource and buries heavy metal contamination (water body, soil) hidden danger.
KCl, NaCl, CaCl is rich in owing to sintering in ash
2, MgCl
2, PbCl
2, CdCl
2deng soluble chloride, in the integrated disposal processing to sintering ash except pyrogenic processing method, other treatment process is all relevant with water.Therefore, above-mentioned soluble chloride major part can be dissolved in water, makes to be rich in chlorion in waste water.If waste water recycles in treating processes, then the chlorine ion concentration in waste water is still to reaching 150000mg/L.
By the comprehensive utilization technique of waste water produced process sintering ash, reclaim potassium, sodium, chlorine and other heavy metal ion in waste water, on the one hand can protection of the environment, turn waste into wealth, for enterprise brings economic benefit; Can make again to draw sintering ash on the other hand and produce smooth and easy carrying out, the resource utilization realizing steel works sintering dust is had important practical significance and actual value.
The current comprehensive utilization technique to the waste water that process sintering ash produces mainly direct condensing crystal is prepared Repone K and utilizes replacement(metathesis)reaction to prepare potassium sulfate technology.University of Science & Technology, Beijing Guo accounts for into the patent of invention (patent No.: 200810101269) " utilize steel enterprise sintering electro-precipitating dust to produce the method for Repone K " waited, the method is under room temperature, adopt tap water, add appropriate SDD to leach under liquid-solid ratio 2/1 ~ 1/1 condition, leaching yield can reach 95% ~ 99.5%.Filter residue after filtration returns sintering circuit after drying, leach liquor heating is concentrated into 3/5 ~ 4/5 of original volume, Slow cooling fractional crystallization Repone K and product, and purity can reach 95% ~ 98%, the total content of magnesium and calcium 0.4% ~ 3%, crystalline mother solution returns the leaching in order to dedusting ash.This method is produced due to production cost, all cannot be widely applied so far.
The Master's thesis " comprehensive utilization of steel works sintering head electro-precipitating dust " of University Of Xiangtan Jiang new people, this technology adds and sinters sulfuric acid and the 2 ‰ hexadecyl brometo de amonios that grey mass ratio is 2%, sintering ash good distribution in water can be made, adopt solid-liquid ratio=1:4, soak time 60min, soaking temperature 30 DEG C, mixing speed 200r/min condition carries out water elution potassium to sintering ash, the eluting rate of potassium can reach 98.70%, and water elution potassium solution is through NH
4hCO
3removal of impurities, activated carbon decolorizing purification, ammonium sulfate replacement(metathesis)reaction, two step evaporative crystallizations can obtain technical grade potassium sulfate, agricultural potassium sulfate and ammonium chloride composite fertilizer respectively, and the total yield of potassium resource can reach 95.54%.The reasons such as this technology is due to complex technical process, and equipment investment is large, and processing cost is high all cannot be widely applied so far.
(number of patent application: 201410493734.8 and number of patent application: all disclose 201410493419.5) " a kind of method utilizing the solid waste containing potassium, chlorion to produce potassium sulfate " such as the patent of invention of Mo Hongbing etc., the method is by adding alcohol Precipitation potassium sulfate, but find in embody rule process, no matter be in storage or concrete application process, this technology, because employ alcohols material, brings certain potential safety hazard to production management.
Summary of the invention
For the deficiency that above-mentioned technology exists, the object of the present invention is to provide a kind of simple, safety, efficient, cost reduces, potassium product quality is high, without the need to using alcohols material to precipitate, and the method being raw material production potassium sulfate with the solid waste containing potassium, chlorion of the potassium nitrogen composite fertilizer of national standard can be met by by-product simultaneously.
Technical scheme of the present invention:
With the solid waste containing potassium, chlorion for a method for raw material production potassium sulfate, comprise the following steps: by the leaching that adds water, in leach liquor, add alkaline matter, soluble carbonate salt removal of impurities, and after concentrating, obtain K
+concentration be the concentrated solution of more than 100g/L; Ammonium sulfate and crystal growth promoters is added in concentrated solution, described crystal growth promoters is the mixture of tripoly phosphate sodium STPP, Secondary ammonium phosphate, magnesium sulfate, urea and sodium sulfate, reaction, obtain potassium sulfate precipitation, solid-liquid separation, obtains potassium sulfate wet slag and filtrate, potassium sulfate wet slag is refining and dry, obtain potassium product, by filtrate wherein by after twice condensing crystal again through super-dry, obtain potassium nitrogen composite fertilizer product;
Wherein, the mass ratio of ammonium sulfate, crystal growth promoters and potassium ion is 1.85 ~ 3.72:0.035 ~ 0.2:1.
The mass ratio of ammonium sulfate, crystal growth promoters and potassium ion is preferably 1.85 ~ 3.72:0.035 ~ 0.1:1.
In crystal growth promoters, the mass ratio of tripoly phosphate sodium STPP, Secondary ammonium phosphate, magnesium sulfate, urea and sodium sulfate is 0.15 ~ 0.32:0.12 ~ 0.20:0.27 ~ 0.35:0.05 ~ 0.10:0.1 ~ 0.27.
The described reaction times is 0.5 ~ 10h.
Described alkaline matter is one or more in sodium hydroxide, potassium hydroxide, sodium carbonate, salt of wormwood, sodium bicarbonate, saleratus, unslaked lime, white lime, adds pH value to 7 ~ 14 removal of impurities of alkaline matter regulator solution.
Described soluble carbonate salt is one or more in sodium carbonate, salt of wormwood, sodium bicarbonate, saleratus, volatile salt, bicarbonate of ammonia.
Described the sintering machine head end electro-precipitating dust, gas ash and/or other dry method collected ash that produce for iron and steel enterprise containing the solid waste of potassium, chlorion.
Add water leaching, makes potassium wherein, chlorion and other soluble impurity ions enter into water, obtain leach liquor and leached mud.
The process adding alkaline matter removal of impurities is: in leach liquor, add that to account for described leach liquor weight be the alkaline matter of 0.08 ~ 5%, and the pH value to 7 of regulator solution ~ 14, carry out removal of impurities.
The process adding soluble carbonate salt removal of impurities is: add after alkaline matter removal of impurities completes, and adds the soluble carbonate salt accounting for described solution weight 0.08 ~ 10% further, carry out removal of impurities in solution after removal of impurities.
K in described leach liquor
2o>=0.8%, Na
2o>=0.1%, Cl
->=1.0%.
K can be realized by method of the present invention
2o total yield is in the product not less than 98.5%, wherein K
2o is the summation that two portions reclaim, and one is the potassium rate of recovery in potassium product; It two is the potassium rate of recovery in potassium nitrogen composite fertilizer product.
Beneficial effect of the present invention
The invention provides a kind of simple, safety, efficient, cost reduces, potassium product quality is high, and the method being raw material production potassium sulfate with the solid waste containing potassium, chlorion of the potassium nitrogen composite fertilizer of national standard can be met by by-product simultaneously.
Production process of the present invention is simple, and be easy to operate continuously, good operation safety, the potassium product quality of recovery is good, and its quality product has exceeded the top grade product standard in the potassium sulfate standard of GB20406-2006.And low production cost of the present invention, invest little, good in economic efficiency, environmentally friendly.
Concrete, contriver is in the continuous research process of the recovery process to the solid waste containing potassium, chlorion, although the potassium sulfate sedimentation effect that the intermediate processing adding alcohol before discovery can obtain, but in concrete industrialized application process, there is various problem, inflammable and explosive due to alcohol self, characteristic excitatory, the most frequently used methyl alcohol also has toxicity and corrodibility; And the alcohols material selected storage request is strict aborning, there is a lot of potential safety hazards in operation inconvenience.Slightly careless and inadvertent, just may cause large security incident (as burning, blast); Staff is easily made to suffer from occupational illness in production process.In the actual production of half a year, just there is the malaise symptoms such as methyl alcohol leaks, operator has headache, feel sick, and caused plant downtime to carry out technological transformation.On this basis, the present invention is inventors herein proposed.
The present invention passes through ammonium sulfate, and add mixture composite of tripoly phosphate sodium STPP, Secondary ammonium phosphate, magnesium sulfate, urea and sodium salt, above-mentioned potential safety hazard can not only be avoided well, also unexpectedly obtain the recovering effect of good potassium sulfate, the quality of the potassium product obtained is good, and the potassium nitrogen composite fertilizer of by-product meets GB15063-2009 national standard, just can direct marketing without the need to adding nitrogen, potassium in addition.And technological operation is simple, smooth and easy, lower to the requirement of operator.
Employing the present invention can steam saving about 0.6 ton (i.e. cost-saving 80 yuan/m than former art breading every cubic metre waste water
3waste water, existing factory processes 48000m every year
3, save production cost more than 3,800,000 yuan every year), the cost saving the water-soluble unrenewable part alcohol of alcohol can be saved, approximately can save more than 800,000 yuan every year.
Accompanying drawing explanation
Fig. 1 is an example of process flow sheet of the present invention.
Embodiment
Following examples are intended to be further described content of the present invention, instead of limit the scope of the invention.
Embodiment 1
1, removal of impurities
To the leaching waste water (main component: K containing potassium, chlorion solid waste
2o content is 5.1%, Cl ion content is 5.9%) in add pH value=7.5 of saturated limewater regulator solution, after stirring removal of impurities 60min, bicarbonate of ammonia (add-on is 0.09% of solution weight) is added again in solution, after stirring removal of impurities 60min, filter, it is for subsequent use that filtrate enters dashpot.
2, concentrated
Removal of impurities liquid in dashpot is joined triple effect falling-film evaporator, is concentrated into K
+content be 128g/L, concentrated solution enters dashpot.
2, potassium sulfate formation reaction
Concentrated solution in dashpot is added reactive tank, add the ammonium sulfate solids (mass ratio=2.7 of ammonium sulfate and potassium ion) of solution weight 34.8% and potassium sulfate crystal growth stimulant (mass ratio=0.052 of promotor and potassium ion of 0.81% simultaneously, crystal promotor forms: the mass ratio of tripoly phosphate sodium STPP, Secondary ammonium phosphate, magnesium sulfate, urea and sodium sulfate is 0.25:0.15:0.32:0.08:0.20), after stirring 300min, filter, filter residue enters potassium sulfate refining step, and filtrate enters condensing crystal operation.
3, potassium sulfate is refined
Potassium sulfate wet slag is added to potassium sulfate refinery pit, adds the saturated limewater of wet slag weight 50% simultaneously, after stirring refining 30min, filter, filter residue enters potassium sulfate drying process, and filtrate enters the first step condensing crystal operation.
4, potassium sulfate is dry
Potassium sulfate wet slag after refining is joined in flash distillation dryer, carries out drying, obtain potassium product (potassium product quality is in table 1.1).
5, the first step condensing crystal
Filtrate joined in triple effect climbing-film evaporator, concentrate, then join in crystallizer and carry out crystallization, filter, filter residue is back to potassium sulfate formation reaction operation, and filtrate enters second step condensing crystal operation.
6, second step condensing crystal
Filtrate is joined in triple effect climbing-film evaporator, concentrate, then join in crystallizer and carry out crystallization, filter, filter residue is potassium, nitrogen composite fertilizer product (potassium, nitrogen composite fertilizer quality product are in table 1.2), and filtrate is back to second step condensing crystal operation.
Table 1.1 is the potassium product qualitative data that embodiment 1 is produced
Table 1.2 is the potassium nitrogen composite fertilizer quality product data that embodiment 1 is produced
| Project | Content |
| N content, % | 21.9 |
| K 2O content, % | 14.1 |
| Total nutrient (N+P 2O 5+K 2O) massfraction/% | 36.0 |
| Moisture (H 2O) massfraction/% | 0.92 |
| Massfraction/the % of chlorion >= | 30 |
Attached: GB15063-2009 composite fertilizer (compound manure) national standard
Requirement
Outward appearance: granular, strip or flaked product, mechanical impurity.
Composite fertilizer (compound manure) should meet the requirement of following table, should meet the indicated value on packaging vessel simultaneously.
The requirement of composite fertilizer (compound manure)
Embodiment 2
1, removal of impurities
To the leaching waste water (main component: main component: K containing potassium, chlorion solid waste
2o content is 5.1%, Cl ion content is 5.9%) in add pH value=9.0 of saturated limewater regulator solution, after stirring removal of impurities 60min, bicarbonate of ammonia (add-on is 0.12% of solution weight) is added again in solution, after stirring removal of impurities 60min, filter, it is for subsequent use that filtrate enters dashpot.
2, concentrated
Removal of impurities liquid in dashpot is joined triple effect falling-film evaporator, is concentrated into K
+content be 128g/L, concentrated solution enters dashpot.
2, potassium sulfate formation reaction
Concentrated solution in dashpot is added reactive tank, add the ammonium sulfate solids (mass ratio=2.7 of ammonium sulfate and potassium ion) of solution weight 34.8% and potassium sulfate crystal growth stimulant (mass ratio=0.078 of promotor and potassium ion of 1.21% simultaneously, crystal promotor form: tripoly phosphate sodium STPP, Secondary ammonium phosphate, magnesium sulfate, urea and mass ratio be 0.25:0.15:0.32:0.08:0.20), after stirring 300min, filter, filter residue enters potassium sulfate refining step, and filtrate enters condensing crystal operation.
3, potassium sulfate is refined
Potassium sulfate wet slag is added to potassium sulfate refinery pit, adds the saturated limewater of wet slag weight 50% simultaneously, after stirring refining 30min, filter, filter residue enters potassium sulfate drying process, and filtrate enters the first step condensing crystal operation.
4, potassium sulfate is dry
Potassium sulfate wet slag after refining is joined in flash distillation dryer, carries out drying, obtain potassium product (potassium product quality is in table 2.1).
5, the first step condensing crystal
Filtrate joined in triple effect climbing-film evaporator, concentrate, then join in crystallizer and carry out crystallization, filter, filter residue is back to potassium sulfate formation reaction operation, and filtrate enters second step condensing crystal operation.
6, second step condensing crystal
Filtrate is joined in triple effect climbing-film evaporator, concentrate, then join in crystallizer and carry out crystallization, filter, filter residue is potassium, nitrogen composite fertilizer product (potassium, nitrogen composite fertilizer quality product are in table 2.2), and filtrate is back to second step condensing crystal operation.
Table 2.1 is the potassium product qualitative data that embodiment 2 is produced
Table 2.2 is the potassium nitrogen composite fertilizer quality product data that embodiment 2 is produced
| Project | Content |
| N content, % | 20.7 |
| K 2O content, % | 14.0 |
| Total nutrient (N+P 2O 5+K 2O) massfraction/% | 34.7 |
| Moisture (H 2O) massfraction/% | 0.87 |
| Massfraction/the % of chlorion >= | 30 |
Embodiment 3
1, removal of impurities
To the leaching waste water (main component: main component: K containing potassium, chlorion solid waste
2o content is 5.1%, Cl ion content is 5.9%) in add pH value=10.0 of saturated limewater regulator solution, after stirring removal of impurities 60min, bicarbonate of ammonia (add-on is 0.15% of solution weight) is added again in solution, after stirring removal of impurities 60min, filter, it is for subsequent use that filtrate enters dashpot.
2, concentrated
Removal of impurities liquid in dashpot is joined triple effect falling-film evaporator, is concentrated into K
+content be 128g/L, concentrated solution enters dashpot.
2, potassium sulfate formation reaction
Concentrated solution in dashpot is added reactive tank, add the ammonium sulfate solids (mass ratio=3.05 of ammonium sulfate and potassium ion) of solution weight 39.15% and potassium sulfate crystal growth stimulant (mass ratio=0.065 of promotor and potassium ion of 1.0% simultaneously, crystal promotor forms: the mass ratio of tripoly phosphate sodium STPP, Secondary ammonium phosphate, magnesium sulfate, urea and sodium sulfate is 0.25:0.15:0.32:0.08:0.20), after stirring 300min, filter, filter residue enters potassium sulfate refining step, and filtrate enters condensing crystal operation.
3, potassium sulfate is refined
Potassium sulfate wet slag is added to potassium sulfate refinery pit, adds the saturated limewater of wet slag weight 50% simultaneously, after stirring refining 30min, filter, filter residue enters potassium sulfate drying process, and filtrate enters the first step condensing crystal operation.
4, potassium sulfate is dry
Potassium sulfate wet slag after refining is joined in flash distillation dryer, carries out drying, obtain potassium product (potassium product quality is in table 3.1).
5, the first step condensing crystal
Filtrate joined in triple effect climbing-film evaporator, concentrate, then join in crystallizer and carry out crystallization, filter, filter residue is back to potassium sulfate formation reaction operation, and filtrate enters second step condensing crystal operation.
6, second step condensing crystal
Filtrate is joined in triple effect climbing-film evaporator, concentrate, then join in crystallizer and carry out crystallization, filter, filter residue is potassium, nitrogen composite fertilizer product (potassium, nitrogen composite fertilizer quality product are in table 3.2), and filtrate is back to second step condensing crystal operation.
Table 3.1 is the potassium product qualitative data that embodiment 3 is produced
Table 3.2 is the potassium nitrogen composite fertilizer quality product data that embodiment 3 is produced
| Project | Content |
| N content, % | 19.8 |
| K 2O content, % | 13.7 |
| Total nutrient (N+P 2O 5+K 2O) massfraction/% | 33.5 |
| Moisture (H 2O) massfraction/% | 1.02 |
| Massfraction/the % of chlorion >= | 30 |
Embodiment 4
1, removal of impurities
To the leaching waste water (main component: main component: K containing potassium, chlorion solid waste
2o content is 5.1%, Cl ion content is 5.9%) in add pH value=10.0 of saturated limewater regulator solution, after stirring removal of impurities 60min, bicarbonate of ammonia (add-on is 0.15% of solution weight) is added again in solution, after stirring removal of impurities 60min, filter, it is for subsequent use that filtrate enters dashpot.
2, concentrated
Removal of impurities liquid in dashpot is joined triple effect falling-film evaporator, is concentrated into K
+content be 128g/L, concentrated solution enters dashpot.
2, potassium sulfate formation reaction
Concentrated solution in dashpot is added reactive tank, add the ammonium sulfate solids (mass ratio=3.05 of ammonium sulfate and potassium ion) of solution weight 39.15% and potassium sulfate crystal growth stimulant (mass ratio=0.065 of promotor and potassium ion of 1.0% simultaneously, crystal promotor forms: the mass ratio of tripoly phosphate sodium STPP, Secondary ammonium phosphate, magnesium sulfate, urea and sodium sulfate is 0.25:0.15:0.32:0.08:0.20), after stirring 300min, filter, filter residue enters potassium sulfate refining step, and filtrate enters condensing crystal operation.
3, potassium sulfate is refined
Potassium sulfate wet slag is added to potassium sulfate refinery pit, adds the saturated limewater of wet slag weight 80% simultaneously, after stirring refining 30min, filter, filter residue enters potassium sulfate drying process, and filtrate enters the first step condensing crystal operation.
4, potassium sulfate is dry
Potassium sulfate wet slag after refining is joined in flash distillation dryer, carries out drying, obtain potassium product (potassium product quality is in table 4.1).
5, the first step condensing crystal
Filtrate joined in triple effect climbing-film evaporator, concentrate, then join in crystallizer and carry out crystallization, filter, filter residue is back to potassium sulfate formation reaction operation, and filtrate enters second step condensing crystal operation.
6, second step condensing crystal
Filtrate is joined in triple effect climbing-film evaporator, concentrate, then join in crystallizer and carry out crystallization, filter, filter residue is potassium, nitrogen composite fertilizer product (potassium, nitrogen composite fertilizer quality product are in table 4.2), and filtrate is back to second step condensing crystal operation.
Table 4.1 is the potassium product qualitative data that embodiment 4 is produced
Table 4.2 is the potassium nitrogen composite fertilizer quality product data that embodiment 4 is produced
| Project | Content |
| N content, % | 20.5 |
| K 2O content, % | 14.2 |
| Total nutrient (N+P 2O 5+K 2O) massfraction/% | 34.7 |
| Moisture (H 2O) massfraction/% | 0.95 |
| Massfraction/the % of chlorion >= | 30 |
Embodiment 5
1, removal of impurities
To the leaching waste water (main component: main component: K containing potassium, chlorion solid waste
2o content is 5.1%, Cl ion content is 5.9%) in add pH value=10.0 of saturated limewater regulator solution, after stirring removal of impurities 60min, bicarbonate of ammonia (add-on is 0.15% of solution weight) is added again in solution, after stirring removal of impurities 60min, filter, it is for subsequent use that filtrate enters dashpot.
2, concentrated
Removal of impurities liquid in dashpot is joined triple effect falling-film evaporator, is concentrated into K
+content be 128g/L, concentrated solution enters dashpot.
2, potassium sulfate formation reaction
Concentrated solution in dashpot is added reactive tank, add the ammonium sulfate solids (mass ratio=3.05 of ammonium sulfate and potassium ion) of solution weight 39.15% and potassium sulfate crystal growth stimulant (mass ratio=0.065 of promotor and potassium ion of 1.0% simultaneously, crystal promotor forms: the mass ratio of tripoly phosphate sodium STPP, Secondary ammonium phosphate, magnesium sulfate, urea and sodium sulfate is 0.17:0.20:0.35:0.1:0.18), after stirring 300min, filter, filter residue enters potassium sulfate refining step, and filtrate enters condensing crystal operation.
3, potassium sulfate is refined
Potassium sulfate wet slag is added to potassium sulfate refinery pit, adds the saturated limewater of wet slag weight 80% simultaneously, after stirring refining 30min, filter, filter residue enters potassium sulfate drying process, and filtrate enters the first step condensing crystal operation.
4, potassium sulfate is dry
Potassium sulfate wet slag after refining is joined in flash distillation dryer, carries out drying, obtain potassium product (potassium product quality is in table 5.1).
5, the first step condensing crystal
Filtrate joined in triple effect climbing-film evaporator, concentrate, then join in crystallizer and carry out crystallization, filter, filter residue is back to potassium sulfate formation reaction operation, and filtrate enters second step condensing crystal operation.
6, second step condensing crystal
Filtrate is joined in triple effect climbing-film evaporator, concentrate, then join in crystallizer and carry out crystallization, filter, filter residue is potassium, nitrogen composite fertilizer product (potassium, nitrogen composite fertilizer quality product are in table 5.2), and filtrate is back to second step condensing crystal operation.
Table 5.1 is the potassium product qualitative data that embodiment 5 is produced
Table 5.2 is the potassium nitrogen composite fertilizer quality product data that embodiment 5 is produced
| Project | Content |
| N content, % | 19.5 |
| K 2O content, % | 14.7 |
| Total nutrient (N+P 2O 5+K 2O) massfraction/% | 34.2 |
| Moisture (H 2O) massfraction/% | 1.0 |
| Massfraction/the % of chlorion >= | 30 |
Embodiment 6
1, removal of impurities
To the leaching waste water (main component: main component: K containing potassium, chlorion solid waste
2o content is 5.1%, Cl ion content is 5.9%) in add pH value=10.0 of saturated limewater regulator solution, after stirring removal of impurities 60min, bicarbonate of ammonia (add-on is 0.15% of solution weight) is added again in solution, after stirring removal of impurities 60min, filter, it is for subsequent use that filtrate enters dashpot.
2, concentrated
Removal of impurities liquid in dashpot is joined triple effect falling-film evaporator, is concentrated into K
+content be 128g/L, concentrated solution enters dashpot.
2, potassium sulfate formation reaction
Concentrated solution in dashpot is added reactive tank, add the ammonium sulfate solids (mass ratio=3.05 of ammonium sulfate and potassium ion) of solution weight 39.15% and potassium sulfate crystal growth stimulant (mass ratio=0.065 of promotor and potassium ion of 1.0% simultaneously, crystal promotor forms: the mass ratio of tripoly phosphate sodium STPP, Secondary ammonium phosphate, magnesium sulfate, urea and sodium sulfate is 0.20:0.18:0.30:0.1:0.22), after stirring 300min, filter, filter residue enters potassium sulfate refining step, and filtrate enters condensing crystal operation.
3, potassium sulfate is refined
Potassium sulfate wet slag is added to potassium sulfate refinery pit, adds the saturated limewater of wet slag weight 80% simultaneously, after stirring refining 30min, filter, filter residue enters potassium sulfate drying process, and filtrate enters the first step condensing crystal operation.
4, potassium sulfate is dry
Potassium sulfate wet slag after refining is joined in flash distillation dryer, carries out drying, obtain potassium product (potassium product quality is in table 6.1).
5, the first step condensing crystal
Filtrate joined in triple effect climbing-film evaporator, concentrate, then join in crystallizer and carry out crystallization, filter, filter residue is back to potassium sulfate formation reaction operation, and filtrate enters second step condensing crystal operation.
6, second step condensing crystal
Filtrate is joined in triple effect climbing-film evaporator, concentrate, then join in crystallizer and carry out crystallization, filter, filter residue is potassium, nitrogen composite fertilizer product (potassium, nitrogen composite fertilizer quality product are in table 6.2), and filtrate is back to second step condensing crystal operation.
Table 6.1 is the potassium product qualitative data that embodiment 6 is produced
Table 6.2 is the potassium nitrogen composite fertilizer quality product data that embodiment 6 is produced
| Project | Content |
| N content, % | 20.1 |
| K 2O content, % | 13.6 |
| Total nutrient (N+P 2O 5+K 2O) massfraction/% | 33.7 |
| Moisture (H 2O) massfraction/% | 0.91 |
| Massfraction/the % of chlorion >= | 30 |
Embodiment 7
1, removal of impurities
To the leaching waste water (main component: K containing potassium, chlorion solid waste
2o content is 5.1%, Cl ion content is 5.9%) in add pH value=10.0 of saturated limewater regulator solution, after stirring removal of impurities 60min, bicarbonate of ammonia (add-on is 0.15% of solution weight) is added again in solution, after stirring removal of impurities 60min, filter, it is for subsequent use that filtrate enters dashpot.
2, concentrated
Removal of impurities liquid in dashpot is joined triple effect falling-film evaporator, is concentrated into K
+content be 128g/L, concentrated solution enters dashpot.
2, potassium sulfate formation reaction
Concentrated solution in dashpot is added reactive tank, add the ammonium sulfate solids (mass ratio=3.05 of ammonium sulfate and potassium ion) of solution weight 39.15% and potassium sulfate crystal growth stimulant (mass ratio=0.065 of promotor and potassium ion of 1.0% simultaneously, crystal promotor forms: the mass ratio of tripoly phosphate sodium STPP, Secondary ammonium phosphate, magnesium sulfate, urea and sodium sulfate is 0.25:0.15:0.27:0.08:0.25), after stirring 300min, filter, filter residue enters potassium sulfate refining step, and filtrate enters condensing crystal operation.
3, potassium sulfate is refined
Potassium sulfate wet slag is added to potassium sulfate refinery pit, adds the saturated limewater of wet slag weight 80% simultaneously, after stirring refining 30min, filter, filter residue enters potassium sulfate drying process, and filtrate enters the first step condensing crystal operation.
4, potassium sulfate is dry
Potassium sulfate wet slag after refining is joined in flash distillation dryer, carries out drying, obtain potassium product (potassium product quality is in table 7.1).
5, the first step condensing crystal
Filtrate joined in triple effect climbing-film evaporator, concentrate, then join in crystallizer and carry out crystallization, filter, filter residue is back to potassium sulfate formation reaction operation, and filtrate enters second step condensing crystal operation.
6, second step condensing crystal
Filtrate is joined in triple effect climbing-film evaporator, concentrate, then join in crystallizer and carry out crystallization, filter, filter residue is potassium, nitrogen composite fertilizer product (potassium, nitrogen composite fertilizer quality product are in table 7.2), and filtrate is back to second step condensing crystal operation.
Table 7.1 is the potassium product qualitative data that embodiment 7 is produced
| Project | K 2O％ | Cl -％ | H 2O％ | Free acid (with | K 2The O rate of recovery |
| H 2SO 4Meter) | ％ | ||||
| Content | 51.4 | 0.62 | 0.5 | 0.02 | 92.0 |
Table 7.2 is the potassium nitrogen composite fertilizer quality product data that embodiment 7 is produced
| Project | Content |
| N content, % | 19.7 |
| K 2O content, % | 13.6 |
| Total nutrient (N+P 2O 5+K 2O) massfraction/% | 33.3 |
| Moisture (H 2O) massfraction/% | 0.97 |
| Massfraction/the % of chlorion >= | 30 |
Embodiment 8
1, removal of impurities
To the leaching waste water (main component: K containing potassium, chlorion solid waste
2o content is 6.2%, Cl ion content is 6.7%) in add pH value=7.5 of saturated limewater regulator solution, after stirring removal of impurities 60min, bicarbonate of ammonia (add-on is 0.09% of solution weight) is added again in solution, after stirring removal of impurities 60min, filter, it is for subsequent use that filtrate enters dashpot.
2, concentrated
Removal of impurities liquid in dashpot is joined triple effect falling-film evaporator, is concentrated into K
+content be 128g/L, concentrated solution enters dashpot.
2, potassium sulfate formation reaction
Concentrated solution in dashpot is added reactive tank, add the ammonium sulfate solids (mass ratio=2.7 of ammonium sulfate and potassium ion) of solution weight 33.8% and potassium sulfate crystal growth stimulant (mass ratio=0.052 of promotor and potassium ion of 0.81% simultaneously, crystal promotor forms: the mass ratio of tripoly phosphate sodium STPP, Secondary ammonium phosphate, magnesium sulfate, urea and sodium sulfate is 0.25:0.15:0.32:0.08:0.20), after stirring 300min, filter, filter residue enters potassium sulfate refining step, and filtrate enters condensing crystal operation.
3, potassium sulfate is refined
Potassium sulfate wet slag is added to potassium sulfate refinery pit, adds the saturated limewater of wet slag weight 50% simultaneously, after stirring refining 30min, filter, filter residue enters potassium sulfate drying process, and filtrate enters the first step condensing crystal operation.
4, potassium sulfate is dry
Potassium sulfate wet slag after refining is joined in flash distillation dryer, carries out drying, obtain potassium product (potassium product quality is in table 8.1).
5, the first step condensing crystal
Filtrate joined in triple effect climbing-film evaporator, concentrate, then join in crystallizer and carry out crystallization, filter, filter residue is back to potassium sulfate formation reaction operation, and filtrate enters second step condensing crystal operation.
6, second step condensing crystal
Filtrate is joined in triple effect climbing-film evaporator, concentrate, then join in crystallizer and carry out crystallization, filter, filter residue is potassium, nitrogen composite fertilizer product (potassium, nitrogen composite fertilizer quality product are in table 8.2), and filtrate is back to second step condensing crystal operation.
Table 8.1 is the potassium product qualitative data that embodiment 8 is produced
Table 8.2 is the potassium nitrogen composite fertilizer quality product data that embodiment 8 is produced
| Project | Content |
| N content, % | 21.3 |
| K 2O content, % | 14.6 |
| Total nutrient (N+P 2O 5+K 2O) massfraction/% | 35.9 |
| Moisture (H 2O) massfraction/% | 0.93 |
| Massfraction/the % of chlorion >= | 30 |
Embodiment 9
1, removal of impurities
To the leaching waste water (main component: K containing potassium, chlorion solid waste
2o content is 6.2%, Cl ion content is 6.7%) in add pH value=7.5 of saturated limewater regulator solution, after stirring removal of impurities 60min, bicarbonate of ammonia (add-on is 0.09% of solution weight) is added again in solution, after stirring removal of impurities 60min, filter, it is for subsequent use that filtrate enters dashpot.
2, concentrated
Removal of impurities liquid in dashpot is joined triple effect falling-film evaporator, is concentrated into K
+content be 135g/L, concentrated solution enters dashpot.
2, potassium sulfate formation reaction
Concentrated solution in dashpot is added reactive tank, add the ammonium sulfate solids (mass ratio=2.0 of ammonium sulfate and potassium ion) of solution weight 32.4% and potassium sulfate crystal growth stimulant (mass ratio=0.052 of promotor and potassium ion of 0.81% simultaneously, crystal promotor forms: the mass ratio of tripoly phosphate sodium STPP, Secondary ammonium phosphate, magnesium sulfate, urea and sodium sulfate is 0.25:0.15:0.32:0.08:0.20), after stirring 300min, filter, filter residue enters potassium sulfate refining step, and filtrate enters condensing crystal operation.
3, potassium sulfate is refined
Potassium sulfate wet slag is added to potassium sulfate refinery pit, adds the saturated limewater of wet slag weight 50% simultaneously, after stirring refining 30min, filter, filter residue enters potassium sulfate drying process, and filtrate enters the first step condensing crystal operation.
4, potassium sulfate is dry
Potassium sulfate wet slag after refining is joined in flash distillation dryer, carries out drying, obtain potassium product (potassium product quality is in table 9.1).
5, the first step condensing crystal
Filtrate joined in triple effect climbing-film evaporator, concentrate, then join in crystallizer and carry out crystallization, filter, filter residue is back to potassium sulfate formation reaction operation, and filtrate enters second step condensing crystal operation.
6, second step condensing crystal
Filtrate is joined in triple effect climbing-film evaporator, concentrate, then join in crystallizer and carry out crystallization, filter, filter residue is potassium, nitrogen composite fertilizer product (potassium, nitrogen composite fertilizer quality product are in table 9.2), and filtrate is back to second step condensing crystal operation.
Table 9.1 is the potassium product qualitative data that embodiment 9 is produced
Table 9.2 is the potassium nitrogen composite fertilizer quality product data that embodiment 9 is produced
| Project | Content |
| N content, % | 22.2 |
| K 2O content, % | 13.2 |
| Total nutrient (N+P 2O 5+K 2O) massfraction/% | 35.4 |
| Moisture (H 2O) massfraction/% | 0.97 |
| Massfraction/the % of chlorion >= | 30 |
Embodiment 10
1, removal of impurities
To the leaching waste water (main component: K containing potassium, chlorion solid waste
2o content is 6.2%, Cl ion content is 6.7%) in add pH value=7.5 of saturated limewater regulator solution, after stirring removal of impurities 60min, bicarbonate of ammonia (add-on is 0.09% of solution weight) is added again in solution, after stirring removal of impurities 60min, filter, it is for subsequent use that filtrate enters dashpot.
2, concentrated
Removal of impurities liquid in dashpot is joined triple effect falling-film evaporator, is concentrated into K
+content be 120g/L, concentrated solution enters dashpot.
2, potassium sulfate formation reaction
Concentrated solution in dashpot is added reactive tank, add the ammonium sulfate solids (mass ratio=2.2 of ammonium sulfate and potassium ion) of solution weight 31.9% and potassium sulfate crystal growth stimulant (mass ratio=0.052 of promotor and potassium ion of 1% simultaneously, crystal promotor forms: the mass ratio of tripoly phosphate sodium STPP, Secondary ammonium phosphate, magnesium sulfate, urea and sodium-chlor is 0.25:0.20:0.30:0.10:0.15), after stirring 300min, filter, filter residue enters potassium sulfate refining step, and filtrate enters condensing crystal operation.
3, potassium sulfate is refined
Potassium sulfate wet slag is added to potassium sulfate refinery pit, and the pH value simultaneously adding wet slag weight 80% is the ammonia soln of 8.5, and after stirring refining 30min, filter, filter residue enters potassium sulfate drying process, and filtrate enters the first step condensing crystal operation.
4, potassium sulfate is dry
Potassium sulfate wet slag after refining is joined in flash distillation dryer, carries out drying, obtain potassium product (potassium product quality is in table 10.1).
5, the first step condensing crystal
Filtrate joined in triple effect climbing-film evaporator, concentrate, then join in crystallizer and carry out crystallization, filter, filter residue is back to potassium sulfate formation reaction operation, and filtrate enters second step condensing crystal operation.
6, second step condensing crystal
Filtrate is joined in triple effect climbing-film evaporator, concentrate, then join in crystallizer and carry out crystallization, filter, filter residue is potassium, nitrogen composite fertilizer product (potassium, nitrogen composite fertilizer quality product are in table 10.2), and filtrate is back to second step condensing crystal operation.
Table 10.1 is the potassium product qualitative data that embodiment 10 is produced
Table 10.2 is the potassium nitrogen composite fertilizer quality product data that embodiment 10 is produced
| Project | Content |
| N content, % | 22.2 |
| K 2O content, % | 13.2 |
| Total nutrient (N+P 2O 5+K 2O) massfraction/% | 35.4 |
| Moisture (H 2O) massfraction/% | 0.97 |
| Massfraction/the % of chlorion >= | 30 |
Comparative example 1
Alkaline matter, carbonate add-on (theoretical addition amount) are not enough, ammonium sulfate add-on is too large.
1, removal of impurities
To the leaching waste water (main component: K containing potassium, chlorion solid waste
2o content is 5.1%, Cl ion content is 5.9%) in add pH value=6.2 of saturated sodium carbonate regulator solution, after stirring removal of impurities 60min, bicarbonate of ammonia (add-on is 0.05% of solution weight) is added again in solution, after stirring removal of impurities 60min, filter, it is for subsequent use that filtrate enters dashpot.
2, concentrated
Removal of impurities liquid in dashpot is joined triple effect falling-film evaporator, is concentrated into K
+content be 128g/L, concentrated solution enters dashpot.
2, potassium sulfate formation reaction
Concentrated solution in dashpot is added reactive tank, add the ammonium sulfate solids (mass ratio=3.75 of ammonium sulfate and potassium ion) of solution weight 48.25% and potassium sulfate crystal growth stimulant (mass ratio=0.065 of promotor and potassium ion of 1.0% simultaneously, crystal promotor forms: the mass ratio of tripoly phosphate sodium STPP, Secondary ammonium phosphate, magnesium sulfate, urea and sodium sulfate is 0.25:0.15:0.32:0.08:0.20), after stirring 300min, filter, filter residue enters potassium sulfate refining step, and filtrate enters condensing crystal operation.
3, potassium sulfate is refined
Potassium sulfate wet slag is added to potassium sulfate refinery pit, adds the saturated limewater of wet slag weight 50% simultaneously, after stirring refining 30min, filter, filter residue enters potassium sulfate drying process, and filtrate enters the first step condensing crystal operation.
4, potassium sulfate is dry
Potassium sulfate wet slag after refining is joined in flash distillation dryer, carries out drying, obtain potassium product.
5, the first step condensing crystal
Filtrate joined in triple effect climbing-film evaporator, concentrate, then join in crystallizer and carry out crystallization, filter, filter residue is back to potassium sulfate formation reaction operation, and filtrate enters second step condensing crystal operation.
6, second step condensing crystal
Filtrate joined in triple effect climbing-film evaporator, concentrate, then join in crystallizer and carry out crystallization, filter, filter residue is potassium nitrogen composite fertilizer product, and filtrate is back to second step condensing crystal operation.
Result
| Project | K 2O％ | Cl -％ | K 2O rate of recovery % |
| Content | 44.9 | 0.91 | 82.1 |
Comparative example 2
Volatile salt add-on (theoretical addition amount) is not enough, ammonium sulfate add-on is excessive.
1, removal of impurities
To the leaching waste water (main component: main component: K containing potassium, chlorion solid waste
2o content is 5.1%, Cl ion content is 5.9%) in add pH value=7.6 of saturated sodium carbonate regulator solution, after stirring removal of impurities 60min, bicarbonate of ammonia (add-on is 0.05% of solution weight) is added again in solution, after stirring removal of impurities 60min, filter, it is for subsequent use that filtrate enters dashpot.
2, concentrated
Removal of impurities liquid in dashpot is joined triple effect falling-film evaporator, is concentrated into K
+content be 128g/L, concentrated solution enters dashpot.
2, potassium sulfate formation reaction
Concentrated solution in dashpot is added reactive tank, add the ammonium sulfate solids (mass ratio=3.75 of ammonium sulfate and potassium ion) of solution weight 48.25% and potassium sulfate crystal growth stimulant (mass ratio=0.065 of promotor and potassium ion of 1.0% simultaneously, crystal promotor forms: the mass ratio of tripoly phosphate sodium STPP, Secondary ammonium phosphate, magnesium sulfate, urea and sodium sulfate is 0.25:0.15:0.32:0.08:0.20), after stirring 300min, filter, filter residue enters potassium sulfate refining step, and filtrate enters condensing crystal operation.
3, potassium sulfate is refined
Potassium sulfate wet slag is added to potassium sulfate refinery pit, adds the saturated limewater of wet slag weight 50% simultaneously, after stirring refining 30min, filter, filter residue enters potassium sulfate drying process, and filtrate enters the first step condensing crystal operation.
4, potassium sulfate is dry
Potassium sulfate wet slag after refining is joined in flash distillation dryer, carries out drying, obtain potassium product.
5, the first step condensing crystal
Filtrate joined in triple effect climbing-film evaporator, concentrate, then join in crystallizer and carry out crystallization, filter, filter residue is back to potassium sulfate formation reaction operation, and filtrate enters second step condensing crystal operation.
6, second step condensing crystal
Filtrate joined in triple effect climbing-film evaporator, concentrate, then join in crystallizer and carry out crystallization, filter, filter residue is potassium, nitrogen composite fertilizer product, and filtrate is back to second step condensing crystal operation.
Result
| Project | K 2O％ | Cl -％ | K 2O rate of recovery % |
| Content | 45.7 | 0.77 | 82.7 |
Comparative example 3
Ammonium sulfate add-on is excessive.
1, removal of impurities
To the leaching waste water (main component: main component: K containing potassium, chlorion solid waste
2o content is 5.1%, Cl ion content is 5.9%) in add pH value=7.65 of saturated sodium carbonate regulator solution, after stirring removal of impurities 60min, bicarbonate of ammonia (add-on is 0.1% of solution weight) is added again in solution, after stirring removal of impurities 60min, filter, it is for subsequent use that filtrate enters dashpot.
2, concentrated
Removal of impurities liquid in dashpot is joined triple effect falling-film evaporator, is concentrated into K
+content be 128g/L, concentrated solution enters dashpot.
2, potassium sulfate formation reaction
Concentrated solution in dashpot is added reactive tank, add the ammonium sulfate solids (mass ratio=3.75 of ammonium sulfate and potassium ion) of solution weight 48.25% and potassium sulfate crystal growth stimulant (mass ratio=0.065 of promotor and potassium ion of 1.0% simultaneously, crystal promotor forms: the mass ratio of tripoly phosphate sodium STPP, Secondary ammonium phosphate, magnesium sulfate, urea and sodium sulfate is 0.25:0.15:0.32:0.08:0.20), after stirring 300min, filter, filter residue enters potassium sulfate refining step, and filtrate enters condensing crystal operation.
3, potassium sulfate is refined
Potassium sulfate wet slag is added to potassium sulfate refinery pit, adds the saturated limewater of wet slag weight 50% simultaneously, after stirring refining 30min, filter, filter residue enters potassium sulfate drying process, and filtrate enters the first step condensing crystal operation.
4, potassium sulfate is dry
Potassium sulfate wet slag after refining is joined in flash distillation dryer, carries out drying, obtain potassium product.
5, the first step condensing crystal
Filtrate joined in triple effect climbing-film evaporator, concentrate, then join in crystallizer and carry out crystallization, filter, filter residue is back to potassium sulfate formation reaction operation, and filtrate enters second step condensing crystal operation.
6, second step condensing crystal
Filtrate joined in triple effect climbing-film evaporator, concentrate, then join in crystallizer and carry out crystallization, filter, filter residue is potassium nitrogen composite fertilizer product, and filtrate is back to second step condensing crystal operation.
Result
| Project | K 2O％ | Cl -％ | K 2O rate of recovery % |
| Content | 46.6 | 0.71 | 82.3 |
Comparative example 4
Ammonium sulfate add-on is too small.
1, removal of impurities
To the leaching waste water (main component: main component: K containing potassium, chlorion solid waste
2o content is 5.1%, Cl ion content is 5.9%) in add pH value=7.65 of saturated sodium carbonate regulator solution, after stirring removal of impurities 60min, bicarbonate of ammonia (add-on is 0.1% of solution weight) is added again in solution, after stirring removal of impurities 60min, filter, it is for subsequent use that filtrate enters dashpot.
2, concentrated
Removal of impurities liquid in dashpot is joined triple effect falling-film evaporator, is concentrated into K
+content be 128g/L, concentrated solution enters dashpot.
2, potassium sulfate formation reaction
Concentrated solution in dashpot is added reactive tank, add the ammonium sulfate solids (mass ratio=1.8 of ammonium sulfate and potassium ion) of solution weight 23.16% and potassium sulfate crystal growth stimulant (mass ratio=0.065 of promotor and potassium ion of 1.0% simultaneously, crystal promotor forms: the mass ratio of tripoly phosphate sodium STPP, Secondary ammonium phosphate, magnesium sulfate, urea and sodium sulfate is 0.25:0.15:0.32:0.08:0.20), after stirring 300min, filter, filter residue enters potassium sulfate refining step, and filtrate enters condensing crystal operation.
3, potassium sulfate is refined
Potassium sulfate wet slag is added to potassium sulfate refinery pit, adds the saturated limewater of wet slag weight 50% simultaneously, after stirring refining 30min, filter, filter residue enters potassium sulfate drying process, and filtrate enters the first step condensing crystal operation.
4, potassium sulfate is dry
Potassium sulfate wet slag after refining is joined in flash distillation dryer, carries out drying, obtain potassium product.
5, the first step condensing crystal
Filtrate joined in triple effect climbing-film evaporator, concentrate, then join in crystallizer and carry out crystallization, filter, filter residue is back to potassium sulfate formation reaction operation, and filtrate enters second step condensing crystal operation.
6, second step condensing crystal
Filtrate joined in triple effect climbing-film evaporator, concentrate, then join in crystallizer and carry out crystallization, filter, filter residue is potassium nitrogen composite fertilizer product, and filtrate is back to second step condensing crystal operation.
Result
| Project | K 2O％ | Cl -％ | K 2O rate of recovery % |
| Content | 50.3 | 0.82 | 50.7 |
Comparative example 5
Potassium sulfate crystal growth stimulant add-on is not enough.
1, removal of impurities
To the leaching waste water (main component: main component: K containing potassium, chlorion solid waste
2o content is 5.1%, Cl ion content is 5.9%) in add pH value=8.0 of saturated limewater regulator solution, after stirring removal of impurities 60min, bicarbonate of ammonia (add-on is 0.12% of solution weight) is added again in solution, after stirring removal of impurities 60min, filter, it is for subsequent use that filtrate enters dashpot.
2, concentrated
Removal of impurities liquid in dashpot is joined triple effect falling-film evaporator, is concentrated into K
+content be 128g/L, concentrated solution enters dashpot.
2, potassium sulfate formation reaction
Concentrated solution in dashpot is added reactive tank, add the ammonium sulfate solids (mass ratio=2.7 of ammonium sulfate and Repone K) of solution weight 34.8% and potassium sulfate crystal growth stimulant (mass ratio=0.026 of promotor and potassium ion of 0.4% simultaneously, crystal promotor forms: the mass ratio of tripoly phosphate sodium STPP, Secondary ammonium phosphate, magnesium sulfate, urea and sodium sulfate is 0.25:0.15:0.32:0.08:0.20), after stirring 300min, filter, filter residue enters potassium sulfate refining step, and filtrate enters condensing crystal operation.
3, potassium sulfate is refined
Potassium sulfate wet slag is added to potassium sulfate refinery pit, adds the saturated limewater of wet slag weight 50% simultaneously, after stirring refining 30min, filter, filter residue enters potassium sulfate drying process, and filtrate enters the first step condensing crystal operation.
4, potassium sulfate is dry
Potassium sulfate wet slag after refining is joined in flash distillation dryer, carries out drying, obtain potassium product.
5, the first step condensing crystal
Filtrate joined in triple effect climbing-film evaporator, concentrate, then join in crystallizer and carry out crystallization, filter, filter residue is back to potassium sulfate formation reaction operation, and filtrate enters second step condensing crystal operation.
6, second step condensing crystal
Filtrate joined in triple effect climbing-film evaporator, concentrate, then join in crystallizer and carry out crystallization, filter, filter residue is potassium nitrogen composite fertilizer product, and filtrate is back to second step condensing crystal operation.
Result
| Project | K 2O％ | Cl -％ | K 2O rate of recovery % |
| Content | 50.9 | 0.76 | 62.3 |
Comparative example 6
The add-on wretched insufficiency of potassium sulfate crystal growth stimulant.
1, removal of impurities
To the leaching waste water (main component: main component: K containing potassium, chlorion solid waste
2o content is 5.1%, Cl ion content is 5.9%) in add pH value=8.0 of saturated limewater regulator solution, after stirring removal of impurities 60min, bicarbonate of ammonia (add-on is 0.12% of solution weight) is added again in solution, after stirring removal of impurities 60min, filter, it is for subsequent use that filtrate enters dashpot.
2, concentrated
Removal of impurities liquid in dashpot is joined triple effect falling-film evaporator, is concentrated into K
+content be 128g/L, concentrated solution enters dashpot.
2, potassium sulfate formation reaction
Concentrated solution in dashpot is added reactive tank, add the ammonium sulfate solids (mass ratio=2.7 of ammonium sulfate and Repone K) of solution weight 34.8% and potassium sulfate crystal growth stimulant (mass ratio=0.0065 of promotor and potassium ion of 0.1% simultaneously, crystal promotor forms: the mass ratio of tripoly phosphate sodium STPP, Secondary ammonium phosphate, magnesium sulfate, urea and sodium sulfate is 0.25:0.15:0.32:0.08:0.20), after stirring 300min, filter, filter residue enters potassium sulfate refining step, and filtrate enters condensing crystal operation.
3, potassium sulfate is refined
Potassium sulfate wet slag is added to potassium sulfate refinery pit, adds the saturated limewater of wet slag weight 50% simultaneously, after stirring refining 30min, filter, filter residue enters potassium sulfate drying process, and filtrate enters the first step condensing crystal operation.
4, potassium sulfate is dry
Potassium sulfate wet slag after refining is joined in flash distillation dryer, carries out drying, obtain potassium product.
5, the first step condensing crystal
Filtrate joined in triple effect climbing-film evaporator, concentrate, then join in crystallizer and carry out crystallization, filter, filter residue is back to potassium sulfate formation reaction operation, and filtrate enters second step condensing crystal operation.
6, second step condensing crystal
Filtrate joined in triple effect climbing-film evaporator, concentrate, then join in crystallizer and carry out crystallization, filter, filter residue is potassium nitrogen composite fertilizer product, and filtrate is back to second step condensing crystal operation.
Result
| Project | K 2O％ | Cl -％ | K 2O rate of recovery % |
| Content | 49.7 | 0.82 | 47.8 |
Comparative example 7
Do not add potassium sulfate crystal growth stimulant.
1, removal of impurities
To the leaching waste water (main component: main component: K containing potassium, chlorion solid waste
2o content is 5.1%, Cl ion content is 5.9%) in add pH value=8.0 of saturated limewater regulator solution, after stirring removal of impurities 60min, bicarbonate of ammonia (add-on is 0.12% of solution weight) is added again in solution, after stirring removal of impurities 60min, filter, it is for subsequent use that filtrate enters dashpot.
2, concentrated
Removal of impurities liquid in dashpot is joined triple effect falling-film evaporator, is concentrated into K
+content be 128g/L, concentrated solution enters dashpot.
2, potassium sulfate formation reaction
Concentrated solution in dashpot is added reactive tank, add the ammonium sulfate solids (mass ratio=2.7 of ammonium sulfate and Repone K) of solution weight 34.8% simultaneously, after stirring 300min, filter, filter residue enters potassium sulfate refining step, and filtrate enters condensing crystal operation.
3, potassium sulfate is refined
Potassium sulfate wet slag is added to potassium sulfate refinery pit, adds the saturated limewater of wet slag weight 50% simultaneously, after stirring refining 30min, filter, filter residue enters potassium sulfate drying process, and filtrate enters the first step condensing crystal operation.
4, potassium sulfate is dry
Potassium sulfate wet slag after refining is joined in flash distillation dryer, carries out drying, obtain potassium product.
5, the first step condensing crystal
Filtrate joined in triple effect climbing-film evaporator, concentrate, then join in crystallizer and carry out crystallization, filter, filter residue is back to potassium sulfate formation reaction operation, and filtrate enters second step condensing crystal operation.
6, second step condensing crystal
Filtrate joined in triple effect climbing-film evaporator, concentrate, then join in crystallizer and carry out crystallization, filter, filter residue is potassium nitrogen composite fertilizer product, and filtrate is back to second step condensing crystal operation.
Result
| Project | K 2O％ | Cl -％ | K 2O rate of recovery % |
| Content | 48.2 | 0.96 | 43.6 |
Comparative example 8
Crystal promotor forms: the mass ratio of tripoly phosphate sodium STPP, Secondary ammonium phosphate, magnesium sulfate, urea and sodium sulfate is 0.1:0.25:0.15:0.2:0.30.
1, removal of impurities
To the leaching waste water (main component: main component: K containing potassium, chlorion solid waste
2o content is 5.1%, Cl ion content is 5.9%) in add pH value=10.0 of saturated limewater regulator solution, after stirring removal of impurities 60min, bicarbonate of ammonia (add-on is 0.15% of solution weight) is added again in solution, after stirring removal of impurities 60min, filter, it is for subsequent use that filtrate enters dashpot.
2, concentrated
Removal of impurities liquid in dashpot is joined triple effect falling-film evaporator, is concentrated into K
+content be 128g/L, concentrated solution enters dashpot.
2, potassium sulfate formation reaction
Concentrated solution in dashpot is added reactive tank, add the ammonium sulfate solids (mass ratio=3.05 of ammonium sulfate and potassium ion) of solution weight 39.15% and the potassium sulfate crystal growth stimulant (mass ratio=0.065 of promotor and potassium ion) of 1.0% simultaneously, after stirring 300min, filter, filter residue enters potassium sulfate refining step, and filtrate enters condensing crystal operation.
3, potassium sulfate is refined
Potassium sulfate wet slag is added to potassium sulfate refinery pit, adds the saturated limewater of wet slag weight 80% simultaneously, after stirring refining 30min, filter, filter residue enters potassium sulfate drying process, and filtrate enters the first step condensing crystal operation.
4, potassium sulfate is dry
Potassium sulfate wet slag after refining is joined in flash distillation dryer, carries out drying, obtain potassium product.
5, the first step condensing crystal
Filtrate joined in triple effect climbing-film evaporator, concentrate, then join in crystallizer and carry out crystallization, filter, filter residue is back to potassium sulfate formation reaction operation, and filtrate enters second step condensing crystal operation.
6, second step condensing crystal
Filtrate joined in triple effect climbing-film evaporator, concentrate, then join in crystallizer and carry out crystallization, filter, filter residue is potassium nitrogen composite fertilizer product, and filtrate is back to second step condensing crystal operation.
Result
Comparative example 9
Crystal promotor forms: the mass ratio of tripoly phosphate sodium STPP, Secondary ammonium phosphate, magnesium sulfate, urea and sodium sulfate is 0.35:0.1:0.2:0.0:0.35.
1, removal of impurities
To the leaching waste water (main component: main component: K containing potassium, chlorion solid waste
2o content is 5.1%, Cl ion content is 5.9%) in add pH value=10.0 of saturated limewater regulator solution, after stirring removal of impurities 60min, bicarbonate of ammonia (add-on is 0.15% of solution weight) is added again in solution, after stirring removal of impurities 60min, filter, it is for subsequent use that filtrate enters dashpot.
2, concentrated
Removal of impurities liquid in dashpot is joined triple effect falling-film evaporator, is concentrated into K
+content be 128g/L, concentrated solution enters dashpot.
2, potassium sulfate formation reaction
Concentrated solution in dashpot is added reactive tank, add the ammonium sulfate solids (mass ratio=3.05 of ammonium sulfate and potassium ion) of solution weight 39.15% and the potassium sulfate crystal growth stimulant (mass ratio=0.065 of promotor and potassium ion) of 1.0% simultaneously, after stirring 300min, filter, filter residue enters potassium sulfate refining step, and filtrate enters condensing crystal operation.
3, potassium sulfate is refined
Potassium sulfate wet slag is added to potassium sulfate refinery pit, adds the saturated limewater of wet slag weight 80% simultaneously, after stirring refining 30min, filter, filter residue enters potassium sulfate drying process, and filtrate enters the first step condensing crystal operation.
4, potassium sulfate is dry
Potassium sulfate wet slag after refining is joined in flash distillation dryer, carries out drying, obtain potassium product.
5, the first step condensing crystal
Filtrate joined in triple effect climbing-film evaporator, concentrate, then join in crystallizer and carry out crystallization, filter, filter residue is back to potassium sulfate formation reaction operation, and filtrate enters second step condensing crystal operation.
6, second step condensing crystal
Filtrate joined in triple effect climbing-film evaporator, concentrate, then join in crystallizer and carry out crystallization, filter, filter residue is potassium nitrogen composite fertilizer product, and filtrate is back to second step condensing crystal operation.
Result
Comparative example 10
Crystal promotor forms: the mass ratio of tripoly phosphate sodium STPP, Secondary ammonium phosphate, magnesium sulfate, urea and sodium sulfate is 0.1:0.3:0.4:0.1:0.10.
1, removal of impurities
To the leaching waste water (main component: main component: K containing potassium, chlorion solid waste
2o content is 5.1%, Cl ion content is 5.9%) in add pH value=10.0 of saturated limewater regulator solution, after stirring removal of impurities 60min, bicarbonate of ammonia (add-on is 0.15% of solution weight) is added again in solution, after stirring removal of impurities 60min, filter, it is for subsequent use that filtrate enters dashpot.
2, concentrated
Removal of impurities liquid in dashpot is joined triple effect falling-film evaporator, is concentrated into K
+content be 128g/L, concentrated solution enters dashpot.
2, potassium sulfate formation reaction
Concentrated solution in dashpot is added reactive tank, add the ammonium sulfate solids (mass ratio=3.05 of ammonium sulfate and potassium ion) of solution weight 39.15% and the potassium sulfate crystal growth stimulant (mass ratio=0.065 of promotor and potassium ion) of 1.0% simultaneously, after stirring 300min, filter, filter residue enters potassium sulfate refining step, and filtrate enters condensing crystal operation.
3, potassium sulfate is refined
Potassium sulfate wet slag is added to potassium sulfate refinery pit, adds the saturated limewater of wet slag weight 80% simultaneously, after stirring refining 30min, filter, filter residue enters potassium sulfate drying process, and filtrate enters the first step condensing crystal operation.
4, potassium sulfate is dry
Potassium sulfate wet slag after refining is joined in flash distillation dryer, carries out drying, obtain potassium product.
5, the first step condensing crystal
Filtrate joined in triple effect climbing-film evaporator, concentrate, then join in crystallizer and carry out crystallization, filter, filter residue is back to potassium sulfate formation reaction operation, and filtrate enters second step condensing crystal operation.
6, second step condensing crystal
Filtrate joined in triple effect climbing-film evaporator, concentrate, then join in crystallizer and carry out crystallization, filter, filter residue is potassium nitrogen composite fertilizer product, and filtrate is back to second step condensing crystal operation.
Result
Comparative example 11
Crystal promotor forms: the mass ratio of Secondary ammonium phosphate, magnesium sulfate, urea and sodium sulfate is 0.20:0.40:0.1:0.30, does not add tripoly phosphate sodium STPP.
1, removal of impurities
To the leaching waste water (main component: main component: K containing potassium, chlorion solid waste
2o content is 5.1%, Cl ion content is 5.9%) in add pH value=10.0 of saturated limewater regulator solution, after stirring removal of impurities 60min, bicarbonate of ammonia (add-on is 0.15% of solution weight) is added again in solution, after stirring removal of impurities 60min, filter, it is for subsequent use that filtrate enters dashpot.
2, concentrated
Removal of impurities liquid in dashpot is joined triple effect falling-film evaporator, is concentrated into K
+content be 128g/L, concentrated solution enters dashpot.
2, potassium sulfate formation reaction
Concentrated solution in dashpot is added reactive tank, add the ammonium sulfate solids (mass ratio=3.05 of ammonium sulfate and potassium ion) of solution weight 39.15% and the potassium sulfate crystal growth stimulant (mass ratio=0.065 of promotor and potassium ion) of 1.0% simultaneously, after stirring 300min, filter, filter residue enters potassium sulfate refining step, and filtrate enters condensing crystal operation.
3, potassium sulfate is refined
Potassium sulfate wet slag is added to potassium sulfate refinery pit, adds the saturated limewater of wet slag weight 80% simultaneously, after stirring refining 30min, filter, filter residue enters potassium sulfate drying process, and filtrate enters the first step condensing crystal operation.
4, potassium sulfate is dry
Potassium sulfate wet slag after refining is joined in flash distillation dryer, carries out drying, obtain potassium product.
5, the first step condensing crystal
Filtrate joined in triple effect climbing-film evaporator, concentrate, then join in crystallizer and carry out crystallization, filter, filter residue is back to potassium sulfate formation reaction operation, and filtrate enters second step condensing crystal operation.
6, second step condensing crystal
Filtrate joined in triple effect climbing-film evaporator, concentrate, then join in crystallizer and carry out crystallization, filter, filter residue is potassium, nitrogen composite fertilizer product, and filtrate is back to second step condensing crystal operation.
Result
Comparative example 12
Crystal promotor forms: the mass ratio of tripoly phosphate sodium STPP, Secondary ammonium phosphate, Tai-Ace S 150 and sodium-chlor is 0.28:0.15:0.32:0.25, does not add urea.
1, removal of impurities
To the leaching waste water (main component: main component: K containing potassium, chlorion solid waste
2o content is 5.1%, Cl ion content is 5.9%) in add pH value=10.0 of saturated limewater regulator solution, after stirring removal of impurities 60min, bicarbonate of ammonia (add-on is 0.15% of solution weight) is added again in solution, after stirring removal of impurities 60min, filter, it is for subsequent use that filtrate enters dashpot.
2, concentrated
Removal of impurities liquid in dashpot is joined triple effect falling-film evaporator, is concentrated into K
+content be 128g/L, concentrated solution enters dashpot.
2, potassium sulfate formation reaction
Concentrated solution in dashpot is added reactive tank, add the ammonium sulfate solids (mass ratio=3.05 of ammonium sulfate and potassium ion) of solution weight 39.15% and the potassium sulfate crystal growth stimulant (mass ratio=0.065 of promotor and potassium ion) of 1.0% simultaneously, after stirring 300min, filter, filter residue enters potassium sulfate refining step, and filtrate enters condensing crystal operation.
3, potassium sulfate is refined
Potassium sulfate wet slag is added to potassium sulfate refinery pit, adds the saturated limewater of wet slag weight 80% simultaneously, after stirring refining 30min, filter, filter residue enters potassium sulfate drying process, and filtrate enters the first step condensing crystal operation.
4, potassium sulfate is dry
Potassium sulfate wet slag after refining is joined in flash distillation dryer, carries out drying, obtain potassium product.
5, the first step condensing crystal
Filtrate joined in triple effect climbing-film evaporator, concentrate, then join in crystallizer and carry out crystallization, filter, filter residue is back to potassium sulfate formation reaction operation, and filtrate enters second step condensing crystal operation.
6, second step condensing crystal
Filtrate joined in triple effect climbing-film evaporator, concentrate, then join in crystallizer and carry out crystallization, filter, filter residue is potassium, nitrogen composite fertilizer product, and filtrate is back to second step condensing crystal operation.
Result
Comparative example 13
Crystal promotor forms: the mass ratio of tripoly phosphate sodium STPP, urea, magnesium sulfate and sodium-chlor is 0.28:0.12:0.35:0.25.
1, removal of impurities
To the leaching waste water (main component: main component: K containing potassium, chlorion solid waste
2o content is 5.1%, Cl ion content is 5.9%) in add pH value=10.0 of saturated limewater regulator solution, after stirring removal of impurities 60min, bicarbonate of ammonia (add-on is 0.15% of solution weight) is added again in solution, after stirring removal of impurities 60min, filter, it is for subsequent use that filtrate enters dashpot.
2, concentrated
Removal of impurities liquid in dashpot is joined triple effect falling-film evaporator, is concentrated into K
+content be 120g/L, concentrated solution enters dashpot.
2, potassium sulfate formation reaction
Concentrated solution in dashpot is added reactive tank, add the ammonium sulfate solids (mass ratio=2.7 of ammonium sulfate and potassium ion) of solution weight 33.62% and the potassium sulfate crystal growth stimulant (mass ratio=0.065 of promotor and potassium ion) of 1.0% simultaneously, after stirring 300min, filter, filter residue enters potassium sulfate refining step, and filtrate enters condensing crystal operation.
3, potassium sulfate is refined
Potassium sulfate wet slag is added to potassium sulfate refinery pit, adds the saturated limewater of wet slag weight 80% simultaneously, after stirring refining 30min, filter, filter residue enters potassium sulfate drying process, and filtrate enters the first step condensing crystal operation.
4, potassium sulfate is dry
Potassium sulfate wet slag after refining is joined in flash distillation dryer, carries out drying, obtain potassium product.
5, the first step condensing crystal
Filtrate joined in triple effect climbing-film evaporator, concentrate, then join in crystallizer and carry out crystallization, filter, filter residue is back to potassium sulfate formation reaction operation, and filtrate enters second step condensing crystal operation.
6, second step condensing crystal
Filtrate joined in triple effect climbing-film evaporator, concentrate, then join in crystallizer and carry out crystallization, filter, filter residue is potassium, nitrogen composite fertilizer product, and filtrate is back to second step condensing crystal operation.
Result
Claims (10)
1. with containing potassium, chlorion solid waste for a method for raw material production potassium sulfate, it is characterized in that, comprise the following steps: by leachings that add water, in leach liquor, add alkaline matter, soluble carbonate salt removal of impurities, and concentrate after, obtain K
+concentration be the concentrated solution of more than 100g/L; Ammonium sulfate and crystal growth promoters is added in concentrated solution, described crystal growth promoters is the mixture of tripoly phosphate sodium STPP, Secondary ammonium phosphate, magnesium sulfate, urea and sodium salt, reaction, obtain potassium sulfate precipitation, solid-liquid separation, obtains potassium sulfate wet slag and filtrate, potassium sulfate wet slag is refining and dry, obtain potassium product, by filtrate wherein by after twice condensing crystal again through super-dry, obtain potassium nitrogen composite fertilizer product;
Wherein, described sodium salt is sodium sulfate or sodium-chlor;
The mass ratio of ammonium sulfate, crystal growth promoters and potassium ion is 1.85 ~ 3.72:0.035 ~ 0.2:1.
2. method according to claim 1, is characterized in that, the mass ratio of ammonium sulfate, crystal growth promoters and potassium ion is 1.85 ~ 3.72:0.035 ~ 0.1:1.
3. method according to claim 1 and 2, it is characterized in that, in crystal growth promoters, the mass ratio of tripoly phosphate sodium STPP, Secondary ammonium phosphate, magnesium sulfate, urea and sodium salt is 0.15 ~ 0.32:0.12 ~ 0.20:0.27 ~ 0.35:0.05 ~ 0.10:0.1 ~ 0.27.
4. method according to claim 3, is characterized in that, the described reaction times is 0.5 ~ 10h.
5. method according to claim 1, it is characterized in that, described alkaline matter is one or more in sodium hydroxide, potassium hydroxide, sodium carbonate, salt of wormwood, sodium bicarbonate, saleratus, unslaked lime, white lime, adds pH value to 7 ~ 14 removal of impurities of alkaline matter regulator solution.
6. method according to claim 1, is characterized in that, described soluble carbonate salt is one or more in sodium carbonate, salt of wormwood, sodium bicarbonate, saleratus, volatile salt, bicarbonate of ammonia.
7. method according to claim 1, is characterized in that, described the sintering machine head end electro-precipitating dust, gas ash and/or other dry method collected ash that produce for iron and steel enterprise containing the solid waste of potassium, chlorion.
8. method according to claim 1 or 5, it is characterized in that, the process adding alkaline matter removal of impurities is: in leach liquor, add that to account for described leach liquor weight be the alkaline matter of 0.08 ~ 5%, and the pH value to 7 of regulator solution ~ 14, carry out removal of impurities.
9. the method according to claim 1 or 6, it is characterized in that, the process adding soluble carbonate salt removal of impurities is: add after alkaline matter removal of impurities completes, and adds the soluble carbonate salt accounting for described solution weight 0.08 ~ 10% further, carry out removal of impurities in solution after removal of impurities.
10. method according to claim 1, is characterized in that, K in leach liquor
2o>=0.8%, Na
2o>=0.1%, Cl
->=1.0%.
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| CN105967212A (en) * | 2016-05-13 | 2016-09-28 | 河北钢铁股份有限公司承德分公司 | Method for preparing potassium sulphate by using potassium salt in sintering machine head electric dust removal ash |
| CN107662931A (en) * | 2016-07-29 | 2018-02-06 | 湖南隆洲驰宇科技有限公司 | It is a kind of that the technique that potassium prepares potassium sulfate is extracted from Potassium waste |
| CN108640128A (en) * | 2018-05-17 | 2018-10-12 | 华北理工大学 | A kind of leaching equipment producing potassium sulfate using metallurgical dust sludge |
| WO2020076778A1 (en) * | 2018-10-08 | 2020-04-16 | Marsulex Environmental Technologies Corporation | Systems and methods for producing potassium sulfate |
| CN111847484A (en) * | 2020-06-17 | 2020-10-30 | 五矿（湖南）铁合金有限责任公司 | Method and system for preparing agricultural potassium sulfate from manganese-series ferroalloy smelting dedusting ash |
| CN113880119A (en) * | 2021-12-09 | 2022-01-04 | 中国科学院过程工程研究所 | Method for preparing potassium sulfate from potassium chloride |
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| CN105967212A (en) * | 2016-05-13 | 2016-09-28 | 河北钢铁股份有限公司承德分公司 | Method for preparing potassium sulphate by using potassium salt in sintering machine head electric dust removal ash |
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| WO2020076778A1 (en) * | 2018-10-08 | 2020-04-16 | Marsulex Environmental Technologies Corporation | Systems and methods for producing potassium sulfate |
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| CN111847484A (en) * | 2020-06-17 | 2020-10-30 | 五矿（湖南）铁合金有限责任公司 | Method and system for preparing agricultural potassium sulfate from manganese-series ferroalloy smelting dedusting ash |
| CN111847484B (en) * | 2020-06-17 | 2022-07-05 | 五矿（湖南）铁合金有限责任公司 | Method and system for preparing agricultural potassium sulfate from manganese-series ferroalloy smelting dedusting ash |
| CN113880119A (en) * | 2021-12-09 | 2022-01-04 | 中国科学院过程工程研究所 | Method for preparing potassium sulfate from potassium chloride |
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