CN102701253A - CO2 mineralization method capable of co-producing potassium-enriched solution by high temperature method - Google Patents
CO2 mineralization method capable of co-producing potassium-enriched solution by high temperature method Download PDFInfo
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- CN102701253A CN102701253A CN2012101887348A CN201210188734A CN102701253A CN 102701253 A CN102701253 A CN 102701253A CN 2012101887348 A CN2012101887348 A CN 2012101887348A CN 201210188734 A CN201210188734 A CN 201210188734A CN 102701253 A CN102701253 A CN 102701253A
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Abstract
The invention discloses a CO2 mineralization method capable of co-producing potassium-enriched solution by a high temperature method, which mainly comprises the following steps of: adequately and evenly mixing smashed potash feldspar-enriched ore power and calcium chloride, and carrying out conversion reaction under the condition that the temperature is not lower than 600 DEG C; putting material which is adequately converted into a reactor, adding water, charging CO2, and carrying out mineralization reaction under the condition that the CO2 partial pressure is 0.3-15MPa, and the temperature is 50-350 DEG C; and charging material liquid which is adequately mineralized into separation equipment to separate the solid from the liquid, wherein the liquid phase is the potassium ion-enriched potassium-enriched solution, and the solid phase is the calcium carbonate-containing mineralized product. The CO2 is mineralized by the technical method disclosed by the invention, and the conversion rate of the potash feldspar component in the ore reaches 96%, so that compared with the highest conversion rate 13% of the existing CO2 mineralization method capable of co-producing the potassium-enriched solution, the conversion rate of the CO2 mineralization method is improved by over 6.3 times.
Description
Technical field
The present invention relates to a kind of CO
2Reduce discharging the mineralising treatment process, particularly relate to a kind of at mineralising CO
2Produce the method for soluble potassium salt in the time of gas.
Background technology
In recent years, Global warming has day by day seriously had influence on the ecotope and the global climate of the earth, comprises that migrating with species extinction, climatic zone of vegetation moved, sea level rise and land is flooded, ocean current changes and El Nino takes place frequently etc.This mainly is by CO
2The warming effect of isothermal chamber gas causes.The 3rd assessment report according to the inter-governmental Committee of Experts of United Nations's climate change (IPCC); The average surface temperature in 20th century whole world has increased by 0.6 ℃; 0.1-0.2m has risen on the SL; If or else take prophylactico-therapeutic measures, when the average surface air temperature in the whole world than 1.4-5.8 ℃ of increase in 1990, the SL is with rising 0.09-0.88m.This will cause serious threat for physical features not high coastal low-lying area and island country.China is greenhouse gases CO
2Discharging big country is that main energy structure has determined that the process industrial of highly energy-consuming is China CO with coal
2The main body of discharging.China CO
2Discharging accounts for world CO
21/ 5 of total emission volumn, and in Future in China in very long period, the energy structure aspect is main basic configuration with continuing to keep coal.As CO
2Discharging big country, China is obligated to CO
2Discharging is carried out strictness control and is administered, and this will produce active influence to solving or alleviating global warming.
At present, developed country is mainly with CO
2Catch with geology and bury as CO
2The emphasis of emission-reduction technology development, but geology is buried the bottleneck that existing risk is its large-scale application of obstruction.In recent years, many large calcic, magnesium salts ore or solid waste utilized have been carried out both at home and abroad, through carbonation reaction fixation of C O
2Process study.Calcic, magnesium salts ore generally are present in the silicate rock of natural formation, for example serpentinite and peridotites.These materials and CO
2Produce such as magnesiumcarbonate (MgCO behind the chemical reaction
3) and lime carbonate (CaCO
3, Wingdale).Because the natural reaction process is slower, therefore need do the enhanced pre-treatment, but this consumes energy very to mineral, adopt this mode to seal CO up for safekeeping by inference
2The power station to consume 60%～180% the energy more.And owing to receive the restriction of technical minable silicate reserves, the ore mineralising is sealed CO up for safekeeping
2Potentiality maybe and pessimistic.At present, CO
2Mineralising is compared with other modes of sealing up for safekeeping, and it is not preponderated on cost, therefore, how to bring into play mineral self economic worth, at CO
2The Chemicals of production high added value in the mineralisation process make CO
2Mineralising is sealed the realization economically feasible up for safekeeping, and these problems are present CO
2Mineralising realizes industrialized bottleneck.
Potash fertilizer is for the China that has world population 1/4th, and is significant self-evident.China is the country of a potassium deficiency, and the water-soluble potassium ore resource only accounts for 0.29% of the world.About 80% potash fertilizer import interdependency obviously is unfavorable for the Sustainable development of China's agricultural.To be higher than the speed increment of nitrogenous fertilizer and phosphate fertilizer, China's potash fertilizer demand is about 1,000 ten thousand tons/a to China's potash fertilizer demand in recent years always, and 7,000,000 tons of needs imports are arranged approximately.Have data to show, the potash fertilizer import volume is to be higher than the speed increase more than 4% every year in recent years.China be world's sylvite particularly potash fertilizer consumption and import rely on one of maximum country, the potash fertilizer consumption accounts for 20% of world's total amount consumed.Import potash fertilizer price decision domestic price has restricted agriculture steady progression to a great extent.But the water-insoluble potassium ore aboundresources of China, total amount surpasses 2 * 10
10T, China once had a lot of research institutions to carry out the research of potassium felspar sand processing potash fertilizer, but did not all have industrial production because of the energy consumption height.If can will produce potash fertilizer and CO
2Mineralising combine, economic benefit and social benefit will significantly be promoted, just can realize suitability for industrialized production.The explored potassium felspar sand mineral resources of China reaches 60 at present, and its reserves reach 79.14 hundred million t approximately, are converted to the potassium oxide reserves by average content and are about 9.20 hundred million t.If be able to exploitation utilization, can satisfy China's potash fertilizer demand at least 100 years.
CO
2The mineralising processing mode is than other CO
2Processing mode has remarkable advantages, and potash fertilizer is again agriculture prodn demand and all very big a kind of fertilizer of breach, and research and development are at CO
2The technology that mineralisation process is produced potash fertilizer has huge social benefit and economic benefit.For this reason, contriver of the present invention has taken the lead in carrying out the CO of the rich potassium solution of coproduction
2The rich potassium solution mineralising of coproduction CO has been developed in the research of mineralising method
2A step process method, and to Patent Office of the People's Republic of China proposed patented claim (applicant: Sichuan University, application number: 201110382112.4, the applying date: on November 25th, 2011).This process method adopts the mineral dust after will pulverizing to place reactor drum, adds calcium chloride solution, feeds CO
2Gas carries out mineralising reaction, CO
2Mineralising generates lime carbonate, and the potassium felspar sand dissolving generates the solution that is rich in potassium ion.Existing CO before this process method has broken through
2The mineralising method is because CO
2The mineralization product added value is low, CO
2The mineralising technology is difficult to the bottleneck of industrializing implementation, for potash fertilizer production provides competent potassium resource.But the insufficient place of this method is, the potassium felspar sand transformation efficiency is lower, and peak rate of conversion also has only 13%, and potassium felspar sand is not fully used, and mineralising efficient is very low.
Summary of the invention:
CO to the rich potassium solution of the coproduction of prior art
2The problem that the mineralising reaction conversion ratio is low, the present invention aims to provide a kind of potassium felspar sand mineralising CO of high conversion
2The method of the rich potassium solution of coproduction simultaneously is to realize CO
2Efficiently seal the efficient utilization of potassium felspar sand up for safekeeping.
Basic Law of the present invention is to be that the natural rock powder of essential mineral composition is a raw material with the potassium felspar sand; And calcium chloride at high temperature reacts between the solid phase; Destroy the stable crystalline structure of potassium felspar sand; Generate active silicoaluminate calcium salt, the solid with main siliceous calcium aluminate is that raw material adds water and feeds CO then
2Reaction is with CO
2Be converted into solid carbonic acid calcium, thereby realize CO
2Gas solidifies, and obtains to be rich in the solution of potassium ion simultaneously.
The CO of the rich potassium solution of pyroprocess coproduction provided by the invention
2The mineralising method mainly comprises following process step:
(1) mineral dust that is rich in potassium felspar sand and the calcium chloride thorough mixing that will pulverize are even, carry out conversion reaction being not less than under 600 ℃ the temperature; Usually under 600 ~ 1000 ℃ temperature, carry out;
(2) place reactor drum to add entry the material after the abundant conversion reaction of step (1), feed CO
2, at CO
2Dividing potential drop is 0.3 ~ 15MPa, and temperature is mineralising reaction under 50 ~ 350 ℃ the condition;
(3) the abundant reacted feed liquid of mineralising of step (2) is sent into separating device and carry out solid-liquid separation, liquid phase is the rich potassium solution that is rich in potassium ion, and solid phase is the solid that contains mineralization product lime carbonate.
In technique scheme of the present invention, being rich in the mineralising powder of potassium felspar sand and the proportioning of calcium chloride in the step (1) can confirm by the stoichiometry of chemical reaction.The mass ratio that is rich in mineralising powder and the calcium chloride of potassium felspar sand generally can be in 0.3 ~ 2 scope.
In technique scheme of the present invention, the conversion of the conversion reaction time in the step (1) to potassium felspar sand has certain influence.Being rich in the mineral dust of potassium felspar sand and the conversion reaction time of calcium chloride is not less than 10min usually, generally in the scope of 10 ~ 200min.
In technique scheme of the present invention, the add-on of water does not have strict restriction in the step (2), as long as the feed liquid that the material after itself and the conversion reaction is made into can make and CO
2Mineralising reaction successfully carry out all can.Mass ratio between the inventory after the add-on of water and step (1) conversion reaction generally can be in 1 ~ 100 scope.
In technique scheme of the present invention, in the step (2), there is certain influence in the reaction times to mineralising efficient.Material after the conversion reaction and CO
2The mineralising reaction times is not less than 10min usually, generally in 10 ~ 200min scope.
In technique scheme of the present invention, can carry out better in order to make reaction, the reaction in the step (2) is preferably carried out having under the stirring condition, and its stir speed (S.S.) can be 50 ~ 1500r/min.
In technique scheme of the present invention, the said mineral dust that is rich in potassium felspar sand preferentially adopts the potassium mass content with K
2The O meter is not less than 5% mineral dust.The potassium-bearing mineral composition comprises at least a in potash feldspar, sanidine and the microline in the mineral dust.
In technique scheme of the present invention, in order to make the reaction of conversion reaction and mineralising, particularly conversion reaction can be carried out better, and the mineral dust particle size preferably is not more than 50 orders.
The CO of the rich potassium solution of pyroprocess coproduction provided by the invention
2The mineralising method is with CO
2Mineralisation process is accomplished in two steps; At first make the mineral dust and the calcium chloride thorough mixing that are rich in potassium felspar sand even; Carry out conversion reaction between the solid phase being not less than under 600 ℃ the high temperature; Destroy the stable crystalline structure of potassium felspar sand, generate active alkaline silicoaluminate calcium salt, then the material after the conversion reaction is added water and feeds CO
2Carry out the mineralising reaction, with CO
2Mineralising is a stable solid lime carbonate, thereby realizes CO
2The gas mineralising, potassium ion gets into liquid phase simultaneously, obtains being rich in the rich potassium solution of potassium ion.Method of the present invention, the conversion reaction of mineral dust under the calcium chloride effect of being rich in potassium felspar sand at high temperature carried out; Because high temperature can be broken the potassium felspar sand stable molecular structure; Help the reaction between itself and the calcium chloride, the potassium component is separated out, therefore improved the transformation efficiency of potassium felspar sand greatly; The transformation efficiency of potassium felspar sand component can be up to 96% in the ore, is the CO of 201110382112.4 the rich potassium solution of coproduction at the application number of preceding proposition than the applicant
2Mineralising method peak rate of conversion 13% has improved 6.3 times, and the potassium felspar sand utilization ratio improves greatly.Again since the mineral dust and the calcium chloride that are rich in potassium felspar sand at high temperature resultant of reaction be active alkaline silicoaluminate calcium salt, by active alkaline silicoaluminate calcium salt and CO
2Gas carries out the mineralising reaction, joins calcium chloride solution than the ore powder that will be rich in potassium felspar sand and directly feeds CO
2Gas carries out the mineralising reaction, has obviously improved CO
2The mineralising efficient of gas.
The CO of the rich potassium solution of pyroprocess coproduction of the present invention
2The mineralising method is implemented, and not only can realize CO
2Mineralising, make CO
2Become the stable calcium carbonate solid from gaseous state, also realized the extraction of potassium element in the water-insoluble potassium ore simultaneously, for potash fertilizer production provides competent potassium resource.
The present invention is in other mineralising methods, and is easy to operate and safe, equipment requirements is low, controlled variable is simple, and production technique is simple; Mineralising efficient significantly promotes than additive method; And generated the product with added value, therefore than other mineralising methods, the present invention has reduced follow-up mineralising CO
2Reaction conditions, it is low that equipment and technology requires, easy realization of industrial production.
Description of drawings:
Accompanying drawing 1 is the technical process schematic block diagram of one embodiment of the invention.
In the accompanying drawings, 1 is the ore disintegrating apparatus; 2 are conversion reaction equipment; The 3rd, CO
2The mineralising conversion unit; The 4th, solid-liquid separating equipment.
Embodiment
To closing embodiment the present invention is specifically described below, so that the personnel of affiliated technical field are to understanding of the present invention.Be necessary what this particularly pointed out to be; Embodiment just is used for the present invention is further specified; Can not be interpreted as restriction to protection domain of the present invention; Affiliated art skilled person to improvement and adjustment that the present invention makes non-intrinsically safe property, should still belong to protection scope of the present invention according to the invention described above content.
With the potassium felspar sand of exploiting out, carry out fragmentation, ball milling makes its particle size less than 200 orders.It is even that the calcium chloride powder of the potassium felspar sand powder of 2.5g and 2.5g is inserted the porcelain boat thorough mixing; Porcelain boat is put into tubular react furnace, be warming up to 800 ℃, take out porcelain boat when naturally cooling to 80 ℃ behind the reaction 60min; Material after the conversion reaction is taken out; The water that adds 75ml is placed in the reaction kettle, is warming up to 150 ℃, feeds CO
2Gas boosts to 4MPa, and stir speed (S.S.) is 250r/min, stops to stir behind the reaction 120min.The question response still is cooled to about 80 ℃, and pressure release to normal pressure is opened reaction kettle, and mineralising reaction back feed liquid is filtered, and obtains containing CaCO
3Solid phase, liquid phase is the rich potassium solution that is rich in potassium ion.The transformation efficiency of potassium felspar sand component is 84.5% in the present embodiment ore.
Embodiment 2
With the potassium felspar sand of exploiting out, carry out fragmentation, ball milling makes its particle size less than 325 orders.It is even that 2.5g potassium felspar sand and 5g calcium chloride powder are inserted the porcelain boat thorough mixing; Porcelain boat is put into tubular react furnace be warming up to 950 ℃; Take out porcelain boat when naturally cooling to 80 ℃ behind the reaction 30min, the material after the conversion reaction is taken out, the water that adds 75ml is placed in the reaction kettle; Be warming up to 150 ℃, feed CO
2Gas boosts to 4MPa, and stir speed (S.S.) is 250r/min, stops to stir behind the reaction 120min.The question response still is cooled to about 80 ℃, and pressure release to normal pressure is opened reaction kettle, and mineralising reaction back feed liquid is filtered, and obtains containing CaCO
3Solid phase, liquid phase is the rich potassium solution that is rich in potassium ion.The transformation efficiency of potassium felspar sand component is 96% in the present embodiment ore
With the potassium felspar sand of exploiting out, carry out fragmentation, ball milling makes its particle size less than 325 orders.It is even that 2.5g potassium felspar sand and 1g calcium chloride powder are inserted the porcelain boat thorough mixing; Porcelain boat is put into tubular react furnace be warming up to 600 ℃; Take out porcelain boat when naturally cooling to 80 ℃ behind the reaction 60min, the material after the conversion reaction is taken out, add the 25ml pure water and be placed in the reaction kettle; Be warming up to 100 ℃, feed CO
2Pressure rises to 2MPa.Stir speed (S.S.) is 250r/min, stops to stir behind the reaction 120min.The question response still is cooled to about 80 ℃, and pressure release to normal pressure is opened reaction kettle, and mineralising reaction back feed liquid is filtered, and obtains containing CaCO
3Solid phase, liquid phase is the rich potassium solution that is rich in potassium ion.The transformation efficiency of potassium felspar sand component is 45% in the present embodiment ore
Embodiment 4:
With the potassium felspar sand of exploiting out, carry out fragmentation, ball milling makes its particle size less than 150 orders.It is even that 2.5g potassium felspar sand and 6g calcium chloride powder are inserted the porcelain boat thorough mixing; Porcelain boat is put into tubular react furnace be warming up to 900 ℃; Take out porcelain boat when naturally cooling to 80 ℃ behind the reaction 30min, the material after the conversion reaction is taken out, the water that adds 75ml is placed in the reaction kettle; Be warming up to 150 ℃, feed CO
2Be adjusted into 5MPa to pressure, hydrothermal temperature is 200 ℃, and stir speed (S.S.) is 500 r/min, and the reaction times is 200min, and the question response still is cooled to about 80 ℃, and pressure release to normal pressure is opened reaction kettle, and mineralising reaction back feed liquid is filtered, and obtains containing CaCO
3Solid phase, liquid phase is the rich potassium solution that is rich in potassium ion.The transformation efficiency of potassium felspar sand component is 65% in the present embodiment ore.
Claims (10)
1. the CO of the rich potassium solution of a pyroprocess coproduction
2The mineralising method is characterized in that mainly comprising following process step:
(1) mineral dust that is rich in potassium felspar sand and the calcium chloride thorough mixing that will pulverize are even, carry out conversion reaction in being not less than under 600 ℃ of temperature;
(2) place reactor drum to add entry the material after the abundant conversion reaction of step (1), feed CO
2, at CO
2Dividing potential drop is 0.3 ~ 15MPa, and temperature is mineralising reaction under 50 ~ 350 ℃ the condition;
(3) the abundant reacted feed liquid of mineralising of step (2) is sent into separating device and carry out solid-liquid separation, liquid phase is the rich potassium solution that is rich in potassium ion, and solid phase is the solid that contains mineralization product lime carbonate.
2. the CO of the rich potassium solution of a kind of pyroprocess coproduction according to claim 1
2The mineralising method is characterized in that, in the step (1), being rich in the mineral dust of potassium felspar sand and the consumption mass ratio of calcium chloride is 0.3 ~ 2.
3. the CO of the rich potassium solution of a kind of pyroprocess coproduction according to claim 1
2The mineralising method is characterized in that, the conversion reaction temperature of step (1) is 600 ~ 1000 ℃.
4. the CO of the rich potassium solution of a kind of pyroprocess coproduction according to claim 1
2The mineralising method is characterized in that, the time of step (1) conversion reaction is no less than 10min.
5. the CO of the rich potassium solution of a kind of pyroprocess coproduction according to claim 1
2The mineralising method is characterized in that, in the step (2), the add-on of water and the mass ratio of the inventory after the conversion reaction are 1 ~ 100.
6. the CO of the rich potassium solution of a kind of pyroprocess coproduction according to claim 1
2The mineralising method is characterized in that, step (2) the mineralising reaction times is no less than 10min.
7. the CO of the rich potassium solution of pyroprocess coproduction according to claim 1
2The mineralising method is characterized in that, step (2) mineralising is reflected under the condition that stir speed (S.S.) is 50 ~ 1500r/min carries out.
8. according to the CO of the rich potassium solution of the described pyroprocess coproduction of one of claim 1 to 7
2The mineralising method is characterized in that, the said mineral dust potassium mass content that is rich in potassium felspar sand is with K
2The O meter is not less than 5%.
9. the CO of the rich potassium solution of pyroprocess coproduction according to claim 8
2The mineralising method is characterized in that, the said mineral dust mineralogical composition that is rich in potassium felspar sand comprises at least a in potash feldspar, sanidine and the microline.
10. the CO of the rich potassium solution of pyroprocess coproduction according to claim 8
2The mineralising method is characterized in that the mineral dust particle diameter that is rich in potassium felspar sand is not more than 50 orders.
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| CN201210188734.8A CN102701253B (en) | 2012-06-08 | 2012-06-08 | CO2 mineralization method capable of co-producing potassium-enriched solution by high temperature method |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102899679A (en) * | 2012-10-24 | 2013-01-30 | 四川大学 | Method for coproducing sulfuric acid by utilizing gypsum mineralized CO2 |
| WO2013075615A1 (en) * | 2011-11-25 | 2013-05-30 | 四川大学 | Method for joint production of potassium-rich solution by mineralizing co2 |
| CN103466661A (en) * | 2013-08-08 | 2013-12-25 | 四川大学 | Method for mineralizing CO2 and co-producing potassium sulfate by using potassium feldspar-calcium sulfate |
| CN103693659A (en) * | 2013-11-11 | 2014-04-02 | 四川大学 | Method for concurrent production of potassium chloride and mineralization fixation of CO2 |
| CN103966622A (en) * | 2014-04-30 | 2014-08-06 | 四川大学 | Method for realizing separation of potassium-rich solution through hydrochloric acid coproduced by utilizing membrane electrolysis technology to mineralize CO2 |
| CN109133076A (en) * | 2018-08-31 | 2019-01-04 | 贺州市骏鑫矿产品有限责任公司 | A kind of potash feldspar deferrization process |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013075615A1 (en) * | 2011-11-25 | 2013-05-30 | 四川大学 | Method for joint production of potassium-rich solution by mineralizing co2 |
| CN102899679A (en) * | 2012-10-24 | 2013-01-30 | 四川大学 | Method for coproducing sulfuric acid by utilizing gypsum mineralized CO2 |
| CN102899679B (en) * | 2012-10-24 | 2015-08-19 | 四川大学 | Utilize gypsum mineralising CO 2the method of co-producing sulfuric acid |
| CN103466661A (en) * | 2013-08-08 | 2013-12-25 | 四川大学 | Method for mineralizing CO2 and co-producing potassium sulfate by using potassium feldspar-calcium sulfate |
| CN103693659A (en) * | 2013-11-11 | 2014-04-02 | 四川大学 | Method for concurrent production of potassium chloride and mineralization fixation of CO2 |
| CN103693659B (en) * | 2013-11-11 | 2015-06-10 | 四川大学 | Method for concurrent production of potassium chloride and mineralization fixation of CO2 |
| CN103966622A (en) * | 2014-04-30 | 2014-08-06 | 四川大学 | Method for realizing separation of potassium-rich solution through hydrochloric acid coproduced by utilizing membrane electrolysis technology to mineralize CO2 |
| CN109133076A (en) * | 2018-08-31 | 2019-01-04 | 贺州市骏鑫矿产品有限责任公司 | A kind of potash feldspar deferrization process |
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