CN1235860C - Process for separating and recovering potash element form Eichhornic crassipes plant - Google Patents
Process for separating and recovering potash element form Eichhornic crassipes plant Download PDFInfo
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- CN1235860C CN1235860C CN 200410012728 CN200410012728A CN1235860C CN 1235860 C CN1235860 C CN 1235860C CN 200410012728 CN200410012728 CN 200410012728 CN 200410012728 A CN200410012728 A CN 200410012728A CN 1235860 C CN1235860 C CN 1235860C
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- potassium
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- tartarus
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Abstract
The present invention discloses a method for separating and recovering potassium elements from eichhornia crassipes, namely water hyacinth. The present invention is characterized in that: lixiviating fresh eichhornia crassipes by using hydrochloric acid with proper concentration, and extruding and separating residues to obtain extract liquor; adding in potassium carbonate solution, filtering out deposits, and passing filtrate through a filling tower; passing clear liquor through a cation-exchange resin with strong acidic to exchange most potassium on a column; washing the potassium on the column by hydrochloric acid with lower concentration, adding in solid potassium carbonate, and neutralizing the acidity of effluent liquor; finally, adding in a precipitator tartaric acid solution, depositing potassium in the effluent liquor to change the effluent liquor into potassium bitartrate, and dehydrating and drying the deposits to obtain the finished potassium hydrogen tartrate. The potassium bitartrate is raw material needed by food industry and pharmaceutical industry. The present invention well eliminates serious eichhornia crassipes weed disaster in environment, recovers rare potassium element resources in environment simultaneously, and is a new way of environmental pollution treatment and resource optimization utilization.
Description
Technical field
The invention belongs to the method for extracting the potassium element from plant, is to separate the Herba Eichhorniae and the method that reclaims the potassium element from a kind of waterplant Herba Eichhorniae specifically, and the plain product of this potassium can be used in foodstuffs industry and pharmaceutical industry.
Technical background
In recent years, Herba Eichhorniae is Herba Eichhorniae (English name Water hyacinth, Eichhornia crassipes), belong to Pontederiaceae, the phoenix eyes Cymbidium, originate in South America, be a kind of in waters all over the world the general a kind of perennial waterplant of growth fast, particularly in the waters of some eutrophication, the reproduction speed of this kind of plant is considerably surprising, (see the Chinese invention patent ublic specification of application, application number: 03104097.7) to such an extent as to form the outstanding problem of current waters environment protection treating.The rapid procreation of Herba Eichhorniae in China's south rivers and lakes in the last few years, because management is not in place, it spreads unchecked the result for stopping up the river course, corrupt after stain water quality hinders other aquatic plants growth, causes disruption of ecological balance.Although biological control is considered to method preferably, up till now, also there is not the effective biological control method of can big area promoting.The most effective the most direct prevention and cure method of water hyacinth is its salvaging to be removed (see the Chinese invention patent ublic specification of application, application number: 03116012.3), but simple the salvaging only pay economically, and do not have output, and in fact this method is difficult to be accepted.Utilize in the mode at existing hyacinth resource utilization, the most generally with Herba Eichhorniae and other material such as pond sludge, animal excrement etc. are carried out aerobic or the anaerobism composting, produce biogas and prepare fertilizer and (see the Chinese invention patent ublic specification of application, application number: 99116385.0 and 03116305.X), the also favourable report of making raw material production food with Herba Eichhorniae (is seen the Chinese invention patent ublic specification of application, application number: 00114569.X) but these tradition to utilize the mode products obtained therefrom to be worth lower, do not had economic benefit to say after offsetting with high salvage expenses, this is the basic reason that Herba Eichhorniae can not thoroughly be administered.
Utilize the waterplant that comprises Herba Eichhorniae to come purifying water body, key is to find the optimal path of comprehensive utilization waterplant resource.Scientific research shows that Herba Eichhorniae contains very abundant potassium element, K in its dry-matter
2The content of O reaches 6%-7%, apparently higher than general plant.According to the literature survey result, useful chemical separation method reclaims noble metal (Water Sci.Technol. such as Ag from the Herba Eichhorniae plant, 1987, Vol.19 (10), Utilization of water hyacinth for removal and recovery of silver from industrial wastewater), but, still be a blank both at home and abroad by the end of so far with the potassium element in separation of chemical separation method and the recycle-water cucurbit plant.If by the potassium element in certain method recovery Herba Eichhorniae, so both can avoid it excessively to multiply the secondary pollution that causes, the eubiosis that keeps water body, has certain learning value in theory, and the improvement and the utilization of resources of Herba Eichhorniae can also be combined, in practical application, can significantly remedy salvage expenses or reduce the cost of other converted productss, can create better economic benefit and social benefit.
Summary of the invention
The objective of the invention is to overcome the defective of prior art, propose a kind of from the Herba Eichhorniae plant, the separation and the method that reclaims the potassium element,, provide a kind of new processing approach for administering Herba Eichhorniae to the pollution of environment simultaneously to effectively utilize the potassium element in the environment.
A kind of method of separating from the Herba Eichhorniae plant and reclaiming the potassium element is characterized in that, earlier with fresh Herba Eichhorniae plant with the lixiviate of 6-8mol/L hydrochloric acid, through extruding separate vat liquor; Add solution of potassium carbonate then, and filter the small amount of precipitate that produces; Remove pigment and water miscible organism with the packing tower that gac is housed; The gained clear liquid makes most of K by storng-acid cation exchange resin
+Be switched on the post; Wash K on the post with the hydrochloric acid of 2-3mol/L
+, add solid carbonic acid potassium neutralized stream again and go out liquid acidity and make neutral, add the precipitation agent tartaric acid solution at last, precipitation K wherein
+Be tartarus; The solution of post precipitation can be used for dissolving tartrate to be used as precipitation agent, is the tartarus finished product with throw out dehydration and drying at last.Gained soluble tartrate of the present invention is the industrial chemicals of food and pharmaceutical industry widespread demand.Therefore the present invention has not only eliminated the Herba Eichhorniae crop smothering that overflows in the environment preferably, has reclaimed the potassium resource of preciousness in the environment simultaneously, is a kind of environmental pollution improvement and waterplant optimizing network resource utilization new way.
More very thin ins and outs are as described in the following step:
1) fresh Herba Eichhorniae is drained to water content 90%, every 100kg adds 2000-2500ml 6-8mol/L hydrochloric acid (commodity) solution, smashs into slurries to pieces;
2) with the slurries lixiviate 0.5h of step 1), filter, be squeezed to the moisture 40-60% of residue, obtain filtrate 1, the placement of this filtrate is spent the night, discard residue with plate-and-frame filter press;
3) with step 2) filtrate 1 in add among 10～15% salt of wormwood (commodity) solution, 9～11L and acidity and precipitation part calcium, magnesium, with sedimentation and filtration, obtain filtrate 2, and discard precipitation;
4) with step 2) filtrate 2 mistake the packing tower absorption pigment and the water miscible organism wherein of gac is housed, obtain filtrate 3, make filtrate 3 contain potassium greater than 0.9%;
5) filtrate 3 is entered storng-acid cation exchange resin with the 1L/h flow, monitored the potassium concn of post solution, work as K
+Be higher than at 0.1% o'clock and stop exchange, discard the pouring fluid;
6) wash K on the post with 2-3mol/L hydrochloric acid 10L
+, obtaining containing potassium is 6-10%, [H
+] be the acid stream fluid of 0.2-0.4mol/L;
7) in the acid stream fluid of step 6), add solid carbonic acid potassium 300-350 gram,, make the K of this solution to pH value of solution=6-8
+Reach l0-12% and be neutral;
8) adding concentration in the solution that step 7) obtains is tartrate (commodity) 5-10L of 50-100%, precipitate K
+Be tartarus, and filter;
9) the throw out dehydration that step 8) is obtained is put 60 ℃ of following oven dry and is the tartarus product.：
Use the present invention prepares tartarus from the Herba Eichhorniae plant economic benefit estimation:
According to relevant market information analysis, tartrate commodity raw material valency is 9000 yuan/ton of Renminbi at present, salt of wormwood commodity raw material valency is 4500 yuan/ton of Renminbi, and hydrochloric acid commodity raw material valency is 600 yuan/ton of Renminbi, and food grade tartarus commodity valency is 12000 yuan/ton of Renminbi.Adopt technology of the present invention, from fresh Herba Eichhorniae plant per ton (is 90% by bright leaf, stem water content), can extract the plain 6kg of potassium, consume salt of wormwood raw material 30kg, tartrate raw material 90kg, hydrochloric acid 70kg, obtaining tartarus is 97kg.Behind the deduction production cost, but 177 yuan of Herba Eichhorniae new output value Renminbi per ton.
Description of drawings
Fig. 1: be process flow sheet of the present invention.
Embodiment
Embodiment 1:
Get the fresh Herba Eichhorniae plant 100kg that drains back water content to 90%, add 8mol/L hydrochloric acid soln 2000ml, smash back lixiviate (reciprocating vibration) half an hour to pieces with the plant refiner, squeeze out steeping fluid with plate-and-frame filter press, about 9000ml, placement is spent the night, the plant residue behind the extrusion impregnating liquid moisture 50%.Add in 10 liters of 12% solution of potassium carbonate and acidity and precipitation part calcium, magnesium through pushing separating obtained vat liquor, with sedimentation and filtration, remove pigment and water miscible organism with the packing tower that gac is housed, fill with glass wool used packing tower bottom, the packing layer height be post high 1/10, the length-to-diameter ratio of adsorption column is 10, and interior dress particle diameter is the activated carbon granule of 2-3mm, and the void tower flow of this packing tower is 0.5dm
3/ min.Gained clear liquid K
+Concentration is 0.98%, and by strong acid cation exchange resin column, flow rate control is about 1L/h then.The significant parameter of resin column is diameter 7cm, and the high 70cm of post, volume are 2.5L, and interior dress 2kg exchange capacity is the 220cmol/kg storng-acid cation exchange resin.Cross the K of post solution
+Concentration is 0.1%, discards the pouring fluid.Wash K on the post with the hydrochloric acid 10L of 2.5mol/L
+, obtain containing potassium 8.0%, [H
+] be the solution of 0.32mol/L.In solution, add 300g solid carbonic acid potassium its effluent liquid acidity that neutralizes and make pH=7-8, contain potassium 10-12%.Add the concentration of using as precipitation agent at last and be 50% tartaric acid solution 10.0L, precipitation K wherein
+Be tartarus, the tartrate that is mixed with 50% concentration with the solution of isolating post precipitation is re-used as the precipitation agent use.Gained precipitation (being tartarus) is product of the present invention with drying under the rearmounted 60 ℃ of temperature of centrifuge dewatering through packing.Through test analysis, present embodiment 1 can obtain the 4845g tartarus, and product purity is 99.5%, and the potassium rate of recovery is 87.4%.
Embodiment 2:
Get the fresh Herba Eichhorniae plant 100kg that drains back water content to 90%, add 6mol/L hydrochloric acid soln 2500ml, smash back lixiviate (reciprocating vibration) half an hour to pieces with the plant refiner, squeeze out steeping fluid with plate-and-frame filter press, about 9000ml, placement is spent the night, the plant residue behind the extrusion impregnating liquid moisture 50%.Add in 10 liters of 12% solution of potassium carbonate and acidity and precipitation part calcium, magnesium through pushing separating obtained vat liquor, with sedimentation and filtration, remove pigment and water miscible organism with the packing tower that gac is housed, fill with glass wool used packing tower bottom, the packing layer height be post high 1/10, the length-to-diameter ratio of adsorption column is 10, and interior dress particle diameter is the activated carbon granule of 2-3mm, and the void tower flow of this packing tower is 0.5dm
3/ min.Gained clear liquid K
+Concentration is 0.98%, and by strong acid cation exchange resin column, flow rate control is about 1L/h then.The significant parameter of resin column is diameter 7cm, and the high 70cm of post, volume are 2.5L, and interior dress 2kg exchange capacity is the 220cmol/kg storng-acid cation exchange resin.The potassium concn of crossing post solution is 0.08%, discards the pouring fluid.Wash K on the post with the hydrochloric acid 12L of 2mol/L
+, obtain containing potassium 8.5%, [H
+] be the solution of 0.29mol/L.In solution, add 300g solid carbonic acid potassium its effluent liquid acidity that neutralizes and make pH=7-8, contain potassium 10-12%.Add the concentration of using as precipitation agent at last and be 100% tartaric acid solution 5.0L, precipitation K wherein
+Be tartarus, the tartrate that is mixed with 100% concentration with the solution of isolating post precipitation is re-used as the precipitation agent use.Gained precipitation (being tartarus) is product of the present invention with drying under the rearmounted 60 ℃ of temperature of centrifuge dewatering through packing.Through test analysis, can obtain the 4893g tartarus in the present embodiment, product purity is 98.5%, the potassium rate of recovery is 88.3%.
Embodiment 3:
Get the fresh Herba Eichhorniae plant 100kg that drains back water content to 90%, add 6mol/L hydrochloric acid soln 2000ml, smash back lixiviate (reciprocating vibration) half an hour to pieces with the plant refiner, squeeze out steeping fluid with plate-and-frame filter press, about 9000ml, placement is spent the night, the plant residue behind the extrusion impregnating liquid moisture 50%.Add in 10 liters of 12% solution of potassium carbonate and acidity and precipitation part calcium, magnesium through pushing separating obtained vat liquor, with sedimentation and filtration, remove pigment and water miscible organism with the packing tower that gac is housed, fill with glass wool used packing tower bottom, the packing layer height be post high 1/10, the length-to-diameter ratio of adsorption column is 10, and interior dress particle diameter is the activated carbon granule of 2-3mm, and the void tower flow of this packing tower is 0.5dm
3/ min.Gained clear liquid potassium concn is 0.98%, and by strong acid cation exchange resin column, flow rate control is about 1L/h then.The significant parameter of resin column is diameter 7cm, and the high 70cm of post, volume are 2.5L, and interior dress 2kg exchange capacity is the 220cmol/kg storng-acid cation exchange resin.The potassium concn of crossing post solution is 0.05%, discards the pouring fluid.Wash K on the post with the hydrochloric acid 8L of 3mol/L
+, obtain containing potassium 8.5%, [H
+] be the solution of 0.29mol/L.In solution, add 300g solid carbonic acid potassium its effluent liquid acidity that neutralizes and make pH=7-8, contain potassium 10-12%.Add the concentration of using as precipitation agent at last and be 50% tartaric acid solution 10.0L, precipitation potassium wherein is tartarus, and the tartrate that is mixed with 50% concentration with the solution of isolating post precipitation is re-used as precipitation agent and uses.Gained precipitation (being tartarus) is product of the present invention with drying under the rearmounted 60 ℃ of temperature of centrifuge dewatering through packing.Through test analysis, can obtain the 4826g tartarus in the present embodiment, product purity is 99.3%, the potassium rate of recovery is 87.1%.
Claims (3)
1, a kind of method of separating from the Herba Eichhorniae plant and reclaiming the potassium element is characterized in that, earlier with fresh Herba Eichhorniae with the lixiviate of 6-8mol/L hydrochloric acid, through extruding separate vat liquor; Add solution of potassium carbonate then, and filter the small amount of precipitate that produces; Remove pigment and water miscible organism with the packing tower that gac is housed; The gained clear liquid makes most of K by storng-acid cation exchange resin
+Be switched on the post; Wash K on the post with the hydrochloric acid of 2-3mol/L
+, add solid carbonic acid potassium neutralized stream again and go out liquid acidity and make neutral, add the precipitation agent tartaric acid solution, precipitation K wherein
+Be tartarus, throw out dehydration and drying are the tartarus finished product.
2, the method for separating and reclaim the potassium element from the Herba Eichhorniae plant according to claim 1 is characterized in that preparing according to the following step:
1) fresh Herba Eichhorniae is drained to water content 90%, every 100kg adds 2000-2500ml 6-8mol/L hydrochloric acid soln, smashs into slurries to pieces;
2) with the slurries lixiviate 0.5h of step 1), filter, be squeezed to the moisture 40-60% of residue, obtain filtrate 1, the placement of this filtrate is spent the night, discard residue with plate-and-frame filter press;
3) with step 2) filtrate 1 in add among 10～15% solution of potassium carbonate, 9～11L and acidity and precipitation part calcium, magnesium, with sedimentation and filtration, obtain filtrate 2, and discard precipitation;
4) filtrate 2 of step 3) is crossed the packing tower that gac is housed, obtain filtrate 3, make filtrate 3 contain potassium greater than 0.9%;
5) filtrate 3 is entered storng-acid cation exchange resin with the 1L/h flow, monitored the K of post solution
+Concentration is worked as K
+Be higher than at 0.1% o'clock and stop exchange, discard the pouring fluid;
6) wash K on the post with 2-3mol/L hydrochloric acid 10L
+Obtaining containing potassium is 6-10%, [H
+] be the acid stream fluid of 0.2-0.4mol/L;
7) in the acid stream fluid of step 6), add solid carbonic acid potassium 300-350 gram, make the K of this solution
+Reach 10-12% and be neutral;
8) adding concentration in the solution that step 7) obtains is the tartrate 5-10L of 50-100%, precipitate K
+Be tartarus, and filter;
9) the throw out dehydration that step 8) is obtained is put 60 ℃ of following oven dry and is the tartarus product.
3, the method for separating and reclaim the potassium element from the Herba Eichhorniae plant according to claim 1 and 2 is characterized in that precipitate K
+For being used to dissolve tartrate, uses the solution behind the tartarus as precipitation agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410012728 CN1235860C (en) | 2004-02-16 | 2004-02-16 | Process for separating and recovering potash element form Eichhornic crassipes plant |
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|---|---|---|---|
| CN 200410012728 CN1235860C (en) | 2004-02-16 | 2004-02-16 | Process for separating and recovering potash element form Eichhornic crassipes plant |
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|---|---|
| CN1560017A CN1560017A (en) | 2005-01-05 |
| CN1235860C true CN1235860C (en) | 2006-01-11 |
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| CN102267892B (en) * | 2011-08-08 | 2013-12-11 | 天津市化学试剂研究所 | Preparation method of potassium hydrogen tartrate used as pH reference reagent |
| CN106489388B (en) * | 2016-11-07 | 2018-09-18 | 浙江理工大学 | A kind of rice seedling transplanter based on ejection-folder alms bowl formula |
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