CN100386129C - Process for preparing potassium sulfate by sea water - Google Patents
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- CN100386129C CN100386129C CNB2005101336896A CN200510133689A CN100386129C CN 100386129 C CN100386129 C CN 100386129C CN B2005101336896 A CNB2005101336896 A CN B2005101336896A CN 200510133689 A CN200510133689 A CN 200510133689A CN 100386129 C CN100386129 C CN 100386129C
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Abstract
The present invention relates to a method of preparing potassium sulfate from seawater, which relates to potassium sulfate preparation and comprises the potassium enriched liquid preparation technology and the finished potassium sulfate preparation technology. In the technology process of preparing potassium enriched liquid, the eluting process that ammonium sulfate solution is used as eluant to elute potassium ions adsorbed on clinoptilolite in an ion exchange column is adopted; in the technology process of preparing finished potassium sulfate, the ammonia educing process that ammonia gas is filled in the potassium enriched liquid in order to educe the potassium sulfate is adopted. The method of the present invention has the advantages of low production cost, wide raw material resources and simple technical process, the present invention can not be limited by raw material production, the production quality achieves the quality index of potassium sulfate or achieves the best quality index of the national standard HG/T3279-1990, and no waste liquid is discharged in the technical process; in addition, zeolite, eluent, ammonia water and brine are respectively recovered and circularly used, and the economic benefit is improved.
Description
Technical field
Technical scheme of the present invention relates to the preparation of potassium sulfate, specifically produces the method for potassium sulfate with seawater.
Technical background
Potassium sulfate is a kind of high-quality chlorideless potassic fertilizer.The potassium sulfate preparation method mainly contains now: with potassium chloride and sulfuric acid is that raw material adopts high-temperature roasting method (Mannheim proeess), with potassium chloride and ammonium sulfate or sodium sulphate is that raw material adopts double decomposition conversion method (CN93111750.X, CN 93104558.4, CN 94118558.3, CN 99115475.4), with the salt lake intercrystalline bittern is that raw material adopts salt pan crystallisation (CN 02143641.X, CN 03134290.6), and be that raw material adopts ion-exchange (CN 02116876.8) with seawater and bittern.With chemical products potassium chloride is the method for raw material, and its production cost directly is subjected to the price of potassium chloride and the restriction in source, again owing to China potassium chloride source is main by import, therefore uses the market competitiveness of these methods production potassium sulfates relatively poor; Though with the salt lake intercrystalline bittern is that the process for producing potassium sulfate production cost of raw material is lower, the potassium reserves in salt lake far can not satisfy domestic demand; It is the ion-exchange process for producing potassium sulfate of raw material that CN 02116876.8 discloses with seawater and bittern, main technical points is to change zeolite into the sodium type earlier, then in post, feed normal temperature seawater, feed normal temperature salt pan bittern again, after removing bittern, feed hot saline saturated bittern again, produce potassium-rich brine, rich potassium bittern is produced in the potassium-rich brine evaporation, again rich potassium bittern and mixing of materials are later carried out the high temperature forced evaporation, through cooling, decomposition, screening and conversion reaction, last Separation of Solid and Liquid gets potassium sulfate again.This method provides new approach for making full use of the sea bittern water resource.But because the raw material bittern of this technology and saturated halogen is all from the preparing salt by working up seawater field, so the potassium sulfate output of this method will be subjected to the restriction of the aquatic output of raw material sea bittern.According to statistics, even the whole utilizations of collectable bittern resource of national sea salt field also can only be produced about 500,000 tons/year of potassium sulfates, far do not satisfy domestic agricultural to the potash fertilizer demand, and the rich potassium bittern of this method separates and produces potassium sulfate and partly adopt high temperature forced evaporation technology, and energy consumption is higher and flow process is more numerous and diverse.At present, the required potassium sulphate fertilizer of China's agricultural still has ten thousand tons/year of 20-30 to lean on import to solve.In a word, the energy-efficient new technology that the development and use natural resources are produced potassium sulfate, the output that improves potassium sulphate fertilizer is very necessary.
Summary of the invention
Technical problem to be solved by this invention is: a kind of method of producing potassium sulfate with seawater is provided.It is that to produce the high shortcoming of the plain raw material sources cost of potassium of potassium sulfate or salt lake intercrystalline bittern be the shortcoming that salt lake potassium reserves that raw material is produced potassium sulfate far can not satisfy the shortcoming of domestic demand or potassium sulfate output is subjected to the restriction of raw material output and energy consumption height, long flow path in the production technology that is raw material with seawater and bittern to raw material that this inventive method has overcome with potassium chloride.
The present invention solves this technical problem the technical scheme that is adopted: the method for producing potassium sulfate with seawater, comprise the preparation technology of rich potassium liquid and the reparation technology of finished product potassium sulfate, it is characterized in that: in the rich potassium liquid technical process of preparation, to have adopted ammonium sulfate be eluant, eluent carries out the wash-out operation of wash-out to being adsorbed on potassium ion on the sodium type clinoptilolite in the ion exchange column; In producing finished product potassium sulfate process process, adopted in rich potassium liquid to feed ammonia and analyse operation with the ammonia of separating out potassium sulfate.
Produce the method for potassium sulfate with seawater, its concrete steps are as follows:
The first step, the preparation technology of rich potassium liquid
At first raw material seawater is fed the ion exchange column of filling sodium type clinoptilolite, the raw material seawater that feeds and the mass ratio of sodium type clinoptilolite are controlled at 6～150: 1, carry out the absorption process of the potassium ion in the seawater under 0～30 ℃, the absorption flow velocity of raw material seawater is controlled at 5～50 meters/hour; With fresh water seawater in the ion exchange column is ejected fully then, be that 20～37% ammonium sulfate eluant, eluents carry out the wash-out operation to the potassium ion in the ion exchange column under 20～100 ℃ of temperature with weight percent concentration again, the mass ratio of eluant, eluent and sodium type clinoptilolite is controlled at 0.40～0.65: 1, make rich potassium liquid; After finishing, the wash-out operation carries out the step for regeneration of ion exchange column, be in the ion exchange column of finishing the wash-out operation, to feed saturated brine under 20～95 ℃ of conditions promptly in temperature, saturated brine feeding amount and sodium type clinoptilolite mass ratio are controlled at 1.8～4.5: 1, and ion exchange column is regenerated; Sodium type clinoptilolite and ammonium salt-containing water obtain regenerating in the step for regeneration of ion exchange column, regeneration sodium type clinoptilolite input recycles, in the ammonium salt-containing water that obtains, then add calcium oxide and carry out the ammonia still process processing, the adding metering of calcium oxide is for containing the molal quantity that waits of ammonia total amount in the salt solution, the ammonia still process temperature is controlled at 100～120 ℃, the ammonia that steams gets byproduct ammoniacal liquor after water absorbs, the gained ammonia concn is controlled at 15～20%, and salt solution is also for recycling after the ammonia still process;
Second step, the reparation technology of finished product potassium sulfate
Ammonia was analysed operation before this, feed ammonia in the rich potassium liquid that promptly in the first step, makes to separate out potassium sulfate, temperature is controlled at 0 ℃～30 ℃, after ammonia concentration reaches weight percent concentration and is 10%～30%, stop ammonia and analyse operation, carry out solid-liquid separation process, the temperature of Separation of Solid and Liquid is controlled at 0 ℃～30 ℃, isolated solid makes the finished product potassium sulfate through the drying process under 105～120 ℃ again after the fresh water washing with this solid weight 5～20%; The liquid phase potassium mother liquor that obtains behind the solid-liquid separation process is heated ammonia still process under 100～120 ℃, the control free ammonia content is less than 0.10% in the liquid phase potassium mother liquor, and the ammonia that steams is used for the ammonia of next circulation and analyses operation; Liquid phase after the ammonia still process is allocated solid ammonium sulfate into, and to make it reach weight percent concentration be 20～37%, as the eluant, eluent of the first step of next circulation.
Producing with seawater in the method for potassium sulfate of the invention described above, the density range of raw material seawater is at 2 ° of B é～25 ° B é.
Producing with seawater in the method for potassium sulfate of the invention described above, the elution flow rate of eluant, eluent is controlled at 3～15 meters/hour in the wash-out operation; The regeneration velocity that feeds saturated brine in the step for regeneration is controlled at 3～15 meters/hour.
The invention has the beneficial effects as follows: the inventive method is compared with the various preparation potassium sulfate methods that with potassium chloride are raw material, has raw material and is easy to get, the advantage that cost is low; The inventive method is compared with the process for producing potassium sulfate that with the salt lake intercrystalline bittern is raw material, has solved the plain raw material sources problem of the potassium of producing potassium sulfate, has overcome the potassium reserves defect of insufficient in salt lake, and the potassium reserves of seawater are inexhaustible; The inventive method is compared with the ion-exchange process for producing potassium sulfate that with seawater and bittern is raw material, because ammonium sulfate is a kind of sufficient cheap industrial chemicals, thereby can not be subjected to the restriction of any raw material output with the output that the inventive method is produced potassium sulfate, and separate the forced evaporation technology that potassium sulfate substitutes high energy consumption with the ammonia precipitation and crystallization, thereby integrated cost is lower.The product potassium sulfate quality that the inventive method makes is good, K
2O 〉=50.0%, Cl
-≤ 1.0%.Its quality reaches the high-class product index among the quality index of import potassium sulphate fertilizer or the HG/T3279-1990 that is up to state standards.In addition, the technical process of the inventive method is simple, does not have discharging of waste liquid in the technical process, zeolite, eluant, eluent, ammoniacal liquor, salt solution are all taked to reclaim, and it is recycled, and have further reduced cost, improved economic benefit, opened up new approach for realizing China's agricultural potassium sulfate self-sufficiency.
Description of drawings
Fig. 1 is the process flow diagram of the inventive method.
The specific embodiment
Fig. 1 shows: raw material seawater is adsorbed with the ion exchange column of filling sodium type clinoptilolite.Seawater after absorption is discharged.By the potassium mother liquor of a water and a last circulation output and the eluant, eluent of ammonium sulfate preparation adsorbate is carried out wash-out.Finish feeding saturated brine in the ion exchange column of filling sodium type clinoptilolite of wash-out operation and regenerated, this saturated brine is that sodium chloride is prepared and got by the recovered brine of cocycle with solid salt.The ammonium salt-containing water that obtains in the step for regeneration adds calcium oxide and carries out the ammonia still process processing, gets byproduct ammoniacal liquor, and gets recovered brine.The rich potassium liquid that the wash-out operation is made carries out ammonia with the ammonia that obtains in the ammonia still process and analyses.The potassium sulfate slurry of separating out carries out Separation of Solid and Liquid.The liquid phase mother liquor that obtains behind the solid-liquid separation process carries out ammonia still process, and the ammonia that steams is used for the ammonia of next circulation and analyses operation, and the potassium mother liquor after the ammonia still process is used for next circulation preparation eluant, eluent.Isolated solid washes drying process with water and makes the finished product potassium sulfate.
Embodiment 1
The first step, the preparation of rich potassium liquid
At first, load among the ion exchange column of φ 30 * 6000mm strap clamp cover, constitute ion interchange unit 4000 gram sodium type using natural clinoptilolites.Feed 20 liters of i.e. raw material concentrated seawaters of 25 ° of B ' e of 24166 grams to ion exchange column with 5 meters/hour flow velocity then, adsorb, adsorption temp is 30 ℃.Containing potassium concn in the raw material concentrated seawater is 4.30 grams per liters, and the absorption back ejects seawater in the ion exchange column fully with fresh water, and containing potassium concn in the seawater of discharge is 1.15 grams per liters.Potassium ion in the seawater is switched in the zeolite.Press the data in the table 1, be mixed with eluant, eluent by potassium mother liquor and solid ammonium sulfate after the ammonia still process of a water and a last circulation, to above-mentioned ion exchange column with 3 meters/hour flow velocity feed temperature be 20 ℃ this eluant, eluent 1500ml promptly 1879 grams carry out wash-out, when obtaining rich potassium liquid 1500ml, stop wash-out.This richness potassium liquid composition is as shown in table 1, contains K
+42.38 grams per liter.Being mixed with temperature with the recovered brine of cocycle and solid salt is 20 ℃ saturated brine, then with 3 meters/hour flow velocity with this salt solution 15000ml promptly 18000 grams feed in the ion exchange column of sodium type using natural clinoptilolites, this moment, zeolite regeneration transferred the sodium type again to, can recycle repeatedly, meanwhile obtain ammonium salt-containing water 15000ml, it contains NH
+ 4Be 7.15 grams per liters.Add calcium oxide 167 grams in ammonium salt-containing water, ammonia still process under 100 ℃ of temperature gets 20% ammoniacal liquor 480 grams, obtains recovered brine 14900ml after the ammonia still process and recycles.Material composition in the potassium enrichment process sees Table 1.
Second step, the producing of finished product potassium sulfate
Feed ammonia after the rich potassium liquid 1500ml that the first step is made is cooled to 0 ℃ and carry out ammonia and analyse, analyse, carry out Separation of Solid and Liquid, separate obtaining potassium sulfate 118 grams, obtain potassium mother liquor 1882 grams at 0 ℃ to stopping ammonia till the weight percent concentration of ammonia reaches 10%.The potassium sulfate of separating out obtains 110 gram potassium sulfate finished products with 6 gram fresh water hydro-peenings after 110 ℃ of dryings.Its quality reaches the quality index of import potassium sulphate fertilizer.The potassium mother liquor that obtains carries out ammonia still process under 100 ℃, free ammonia content stops ammonia still process less than 0.10% in liquid phase potassium mother liquor.Obtain circulating mother liquor 1680 grams after the ammonia still process, ammonia steam 202 grams that steam enter next circulation ammonia and analyse.Material component in the potassium sulfate separation process sees Table 2.
Table 1 potassium enrichment process material component table
Table 2 potassium sulfate separation process material component table
Embodiment 2
The first step, the preparation of rich potassium liquid
At first, load among the ion exchange column of φ 30 * 6000mm strap clamp cover, constitute ion interchange unit 4000 gram sodium type using natural clinoptilolites.Feed 600 liters of i.e. raw material seawater of 2 ° of B ' e of 609 kilograms to ion exchange column with 50 meters/hour flow velocity then, adsorb, adsorption temp is 0 ℃.Containing potassium concn in the raw material seawater is 0.32 grams per liter, and the absorption back ejects seawater in the ion exchange column fully with fresh water, and containing potassium concn in the seawater of discharge is 0.16 grams per liter.Potassium ion in the seawater is switched in the zeolite.Press the data in the table 3, be mixed with eluant, eluent by potassium mother liquor and solid ammonium sulfate after the ammonia still process of a water and a last circulation, to above-mentioned ion exchange column with 8 meters/hour flow velocity feed temperature be 100 ℃ this eluant, eluent 2000ml promptly 2586 grams carry out wash-out, obtain rich potassium liquid 1600ml.This richness potassium liquid composition is as shown in table 3, contains K
+56.20 grams per liter.Being mixed with temperature with the recovered brine of cocycle and solid salt is 95 ℃ saturated brine, then with 15 meters/hour flow velocity with temperature be 95 ℃ saturated brine 6000ml promptly 7200 grams feed in the ion exchange column of sodium type using natural clinoptilolites, this moment, zeolite regeneration transferred the sodium type again to, can recycle repeatedly, meanwhile obtain ammonium salt-containing water 6000ml, it contains NH
+ 4Be 13.56 grams per liters.In ammonium salt-containing water, add calcium oxide 127 grams,, obtain 15% ammoniacal liquor 488 grams, obtain recovered brine 5900ml after the ammonia still process and recycle 120 ℃ of ammonia still processs.Material composition in the potassium enrichment process sees Table 3.
Second step, the producing of finished product potassium sulfate
Feed ammonia after the rich potassium liquid 1600ml that the first step is made is cooled to 20 ℃ and carry out ammonia and analyse, analyse, carry out Separation of Solid and Liquid, separate obtaining potassium sulfate 184 grams, obtain potassium mother liquor 2846 grams at 20 ℃ to stopping ammonia till the weight percent concentration of ammonia reaches 30%.The potassium sulfate of separating out obtains 175 gram potassium sulfate finished products with 18 gram fresh water hydro-peenings after 105 ℃ of dryings.Its quality reaches the high-class product standard index (K among the national sector standard HG/T3279-1990
2O 〉=50%, Cl
-≤ 1.0%, H
2O≤1.0%).The potassium mother liquor that obtains carries out ammonia still process under 110 ℃, free ammonia content stops ammonia still process less than 0.10% in liquid phase potassium mother liquor.Obtain circulating mother liquor 1850 grams after the ammonia still process, ammonia steam 900 grams that steam enter next circulation ammonia and analyse.Material component in the potassium sulfate separation process sees Table 4.
Table 3 potassium enrichment process material component table
Table 4 potassium sulfate separation process material component table
Embodiment 3
The first step, the preparation of rich potassium liquid
At first, load among the ion exchange column of φ 30 * 6000mm strap clamp cover, constitute ion interchange unit 4000 gram sodium type using natural clinoptilolites.Feed 100 liters of i.e. raw material concentrated seawaters of 109 kilograms of 12 ° of B ' e to ion exchange column with 15 meters/hour flow velocity then, adsorb, adsorption temp is 15 ℃.Containing potassium concn in the raw material seawater is 1.52 grams per liters, and the absorption back ejects seawater in the ion exchange column fully with fresh water, and containing potassium concn in the seawater of discharge is 0.75 grams per liter.Potassium ion in the seawater is switched in the zeolite.Press the data in the table 5, be mixed with eluant, eluent by mother liquor and solid ammonium sulfate after the ammonia still process of a water and a last circulation, to above-mentioned ion exchange column with 15 meters/hour flow velocity feed temperature be 70 ℃ this eluant, eluent 1250ml promptly 1610 kilograms carry out wash-out, obtain rich potassium liquid 1250ml.This richness potassium liquid composition is as shown in table 5, contains K
+53.67 grams per liter.Being mixed with temperature with the recovered brine of cocycle and solid salt is 50 ℃ saturated brine, be in 50 ℃ the saturated brine 12000ml ion exchange column that promptly 14400 kilograms feed sodium type using natural clinoptilolites with temperature with 10 meters/hour flow velocity then, this moment, zeolite regeneration transferred the sodium type again to, can recycle repeatedly, meanwhile obtain ammonium salt-containing water 11000ml, it contains NH
+ 4Be 10.58 grams per liters.In ammonium salt-containing water, add calcium oxide 181 grams,, obtain 18% ammoniacal liquor 666 grams, obtain recovered brine 11900ml after the ammonia still process and recycle 110 ℃ of ammonia still processs.Material composition in the potassium enrichment process sees Table 5.
Second step, the producing of finished product potassium sulfate
Feed ammonia after the rich potassium liquid 1250ml that the first step is made is cooled to 30 ℃ and carry out ammonia and analyse, analyse, carry out Separation of Solid and Liquid, separate obtaining potassium sulfate 130 grams, obtain potassium mother liquor 1928 grams at 30 ℃ to stopping ammonia till the weight percent concentration of ammonia reaches 20%.The potassium sulfate of separating out obtains 125 gram potassium sulfate finished products with 26 gram fresh water hydro-peenings after 120 ℃ of dryings.Its quality reaches the high-class product standard index (K among the national sector standard HG/T3279-1990
2O 〉=50%, Cl
-≤ 1.0%, H
2O≤1.0%).The potassium mother liquor that obtains carries out ammonia still process under 120 ℃, free ammonia content stops ammonia still process less than 0.10% in liquid phase potassium mother liquor.Obtain circulating mother liquor 1516 grams after the ammonia still process, ammonia steam 405 grams that steam enter next circulation ammonia and analyse.Material component in the potassium sulfate separation process sees Table 6.
Table 5 potassium enrichment process material component table
Table 6 potassium sulfate separation process material component table
% in the foregoing description table 2,4,6 is meant weight percent concentration.
Claims (4)
1. produce the method for potassium sulfate with seawater, comprise the preparation technology of rich potassium liquid and the reparation technology of finished product potassium sulfate, in the rich potassium liquid technical process of preparation, to have adopted ammonium sulfate be eluant, eluent carries out the wash-out operation of wash-out to being adsorbed on potassium ion on the sodium type clinoptilolite in the ion exchange column; In producing finished product potassium sulfate process process, adopted in rich potassium liquid to feed ammonia and analyse operation with the ammonia of separating out potassium sulfate, it is characterized in that concrete steps are as follows:
The first step, the preparation technology of rich potassium liquid
At first raw material seawater is fed the ion exchange column of filling sodium type clinoptilolite, the raw material seawater that feeds and the mass ratio of sodium type clinoptilolite are controlled at 6～150: 1, carry out the absorption process of the potassium ion in the seawater under 0～30 ℃, the absorption flow velocity of raw material seawater is controlled at 5～50 meters/hour; With fresh water seawater in the ion exchange column is ejected fully then, be that 20～37% ammonium sulfate eluant, eluents carry out the wash-out operation to the potassium ion in the ion exchange column under 20～100 ℃ of temperature with weight percent concentration again, the mass ratio of eluant, eluent and sodium type clinoptilolite is controlled at 0.40～0.65: 1, make rich potassium liquid; After finishing, the wash-out operation carries out the step for regeneration of ion exchange column, be in the ion exchange column of finishing the wash-out operation, to feed saturated brine under 20～95 ℃ of conditions promptly in temperature, saturated brine feeding amount and sodium type clinoptilolite mass ratio are controlled at 1.8～4.5: 1, and ion exchange column is regenerated; Sodium type clinoptilolite and ammonium salt-containing water obtain regenerating in the step for regeneration of ion exchange column, regeneration sodium type clinoptilolite input recycles, in the ammonium salt-containing water that obtains, then add calcium oxide and carry out the ammonia still process processing, the adding metering of calcium oxide is for containing the molal quantity that waits of ammonia total amount in the salt solution, the ammonia still process temperature is controlled at 100～120 ℃, the ammonia that steams gets byproduct ammoniacal liquor after water absorbs, the gained ammonia concn is controlled at 15～20%, and salt solution is also for recycling after the ammonia still process;
Second step, the reparation technology of finished product potassium sulfate
Ammonia was analysed operation before this, feed ammonia in the rich potassium liquid that promptly in the first step, makes to separate out potassium sulfate, temperature is controlled at 0 ℃～30 ℃, after ammonia concentration reaches weight percent concentration and is 10%～30%, stop ammonia and analyse operation, carry out solid-liquid separation process, the temperature of Separation of Solid and Liquid is controlled at 0 ℃～30 ℃, isolated solid makes the finished product potassium sulfate through the drying process under 105～120 ℃ again after the fresh water washing with this solid weight 5～20%; The liquid phase potassium mother liquor that obtains behind the solid-liquid separation process is heated ammonia still process under 100～120 ℃, the control free ammonia content is less than 0.10% in the liquid phase potassium mother liquor, and the ammonia that steams is used for the ammonia of next circulation and analyses operation; Liquid phase after the ammonia still process is allocated solid ammonium sulfate into, and to make it reach weight percent concentration be 20～37%, as the eluant, eluent of the first step of next circulation.
2. produce the method for potassium sulfate according to claim 1 is described with seawater, it is characterized in that: the density range of raw material seawater is at 2 ° of B é～25 ° B é.
3. produce the method for potassium sulfate according to claim 1 is described with seawater, it is characterized in that: the eluant, eluent elution flow rate in the wash-out operation is controlled at 3～15 meters/hour.
4. produce the method for potassium sulfate according to claim 1 is described with seawater, it is characterized in that: the regeneration velocity that feeds saturated brine in the step for regeneration is controlled at 3～15 meters/hour.
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| CN101229922B (en) * | 2007-01-23 | 2010-08-25 | 成都理工大学 | Method for abstracting potassium from straw by microwave technique |
| CN101323457B (en) * | 2008-07-25 | 2010-04-14 | 国家海洋局天津海水淡化与综合利用研究所 | Method for preparing potassium muriate by using sea water |
| CN102826574B (en) * | 2012-09-06 | 2014-02-26 | 河北工业大学 | Method for extracting potassium from sea water by using continuous ion exchange method |
| CN105692656A (en) * | 2016-01-13 | 2016-06-22 | 中国海洋大学 | Integrated technology and equipment for bitter bittern resource utilization |
| CN105523813A (en) * | 2016-01-30 | 2016-04-27 | 上海力脉环保设备有限公司 | Method for preparing NPK compound fertilizer from potash salt slurry |
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| 沸石法海水提取硫酸钾新工艺的研究. 刘景府，15-16、25-43页，河北工业大学. 2005 |
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