CN102701253B - 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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- CN102701253B CN102701253B CN201210188734.8A CN201210188734A CN102701253B CN 102701253 B CN102701253 B CN 102701253B CN 201210188734 A CN201210188734 A CN 201210188734A CN 102701253 B CN102701253 B CN 102701253B
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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 mineralising treatment process, particularly relate to a kind of at mineralising CO
2when gas, produce the method for soluble potassium salt.
Background technology
In recent years, Global warming has day by day seriously had influence on 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 with El Nino and take place frequently etc.This is mainly by CO
2the warming effect of isothermal chamber gas causes.According to the 3rd of the inter-governmental Committee of Experts of United Nations's climate change (IPCC) the assessment report, the average surface temperature of 20 th Century has increased by 0.6 ℃, the sea level 0.1-0.2m that risen, if or else take prophylactico-therapeutic measures, when the average surface air temperature in the whole world increased 1.4-5.8 ℃ than 1990, sea level is by rising 0.09-0.88m.This will cause serious threat for the not high coastal low laying areas of physical features and island country.China is greenhouse gases CO
2discharge big country, has determined that take coal as main energy structure the process industrial of highly energy-consuming is China CO
2the main body of discharge.China CO
2discharge accounts for world CO
21/ 5 of total emission volumn, and within Future in China very long period, it is main basic configuration that energy structure aspect will continue to maintain coal.As CO
2discharge big country, China is obligated to CO
2discharge is strictly controlled and administers, and this will produce active influence to solving or alleviating global warming.
At present, developed country is mainly with CO
2catch with Geological storage as CO
2the emphasis of emission-reduction technology development, but the existing risk of Geological storage is to hinder the bottleneck of its large-scale application.In recent years, many large calcic, magnesium salts ore or solid waste utilized have been carried out both at home and abroad, by carbonation reaction fixation of C O
2process study.Calcic, magnesium salts ore are generally present in the silicate rock of natural formation, for example serpentinite and peridotites.These materials and CO
2after chemical reaction, produce such as magnesiumcarbonate (MgCO
3) and calcium carbonate (CaCO
3, Wingdale).Because natural reaction process is slower, therefore need mineral to do enhancement pre-treatment, but this consumes energy very much, adopt by inference and seal in this way CO up for safekeeping
2power station to consume 60%～180% the energy more.And owing to being subject to technical minable silicate storage quantitative limitation, ore mineralising is sealed CO up for safekeeping
2potentiality may and pessimistic.At present, CO
2mineralising is compared with other seal mode up for safekeeping, and it does not preponderate on cost, therefore, how to bring into play mineral self economic worth, at CO
2in mineralisation process, the Chemicals of production high added value, make CO
2mineralising is sealed up for safekeeping and is realized economically feasible, and these problems are current CO
2mineralising realizes industrialized bottleneck.
Potash fertilizer is for the China that has world population 1/4th, significant self-evident.China is the country of a potassium deficiency, 0.29% of the water-soluble potassium ore resource Jin Zhan world.Approximately 80% potash fertilizer import interdependency is obviously unfavorable for the Sustainable development of China's agricultural.China's potash fertilizer demand is always with the speed increment higher than nitrogenous fertilizer and phosphate fertilizer, and China's potash fertilizer demand is about 1,000 ten thousand tons/a in recent years, approximately has 7,000,000 tons of needs imports.Have data to show, in recent years potash fertilizer import volume with annual higher than more than 4% speed increase.China be world's sylvite particularly potash fertilizer consumption and import rely on one of maximum country, 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 China's insoluble potassium ore stone aboundresources, total amount exceedes 2 × 10
10t, China once had a lot of research institutions to carry out the research of potassium felspar sand processing potash fertilizer, but all there is no industrial production because energy consumption is high.If can will produce potash fertilizer and CO
2mineralising combine, will make economic benefit and social benefit significantly promote, just can realize suitability for industrialized production.The explored potassium felspar sand mineral resources of China reaches 60 at present, and its reserves approximately reach 79.14 hundred million t, be converted to potassium oxide reserves be about 9.20 hundred million t by average content.If exploited utilization, can at least meet China's potash fertilizer demand 100 years.
CO
2mineralising processing mode is compared with other CO
2processing mode has obvious advantage, and potash fertilizer is again all very large a kind of fertilizer of agriculture production demand and 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, the present inventor has taken the lead in carrying out the CO of the rich potassium solution of coproduction
2the research of mineralising method, has developed the rich potassium solution mineralising of coproduction CO
2a step process method, and to Patent Office of the People's Republic of China, patent application (applicant: Sichuan University, application number: 201110382112.4, applying date: on November 25th, 2011) has been proposed.This processing method adopts the mineral dust after pulverizing is placed in to reactor, adds calcium chloride solution, passes into CO
2gas carries out mineralising reaction, CO
2mineralising generates calcium carbonate, and potassium felspar sand dissolves and generates the solution that is rich in potassium ion.Existing CO before this processing method has broken through
2mineralising method is due to CO
2mineralization product added value is low, CO
2mineralising technology is difficult to the bottleneck of industrializing implementation, produces sufficient potassium resource is provided for potash fertilizer.But the place of the method deficiency is, potassium felspar sand transformation efficiency is lower, and peak rate of conversion also only has 13%, and potassium felspar sand is not fully used, and mineralising efficiency is very low.
Summary of the invention:
For the CO of the rich potassium solution of the coproduction of prior art
2the problem that 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, to realize CO
2efficiently seal up for safekeeping, the efficient utilization of potassium felspar sand.
Basic Law of the present invention is that natural rock powder take potassium felspar sand as essential mineral composition is as raw material, and calcium chloride at high temperature reacts between solid phase, destroy the stable crystalline structure of potassium felspar sand, generate active silicoaluminate calcium salt, then add water and pass into CO take the solid of main siliceous calcium aluminate as raw material
2reaction, by CO
2be converted into solid carbonic acid calcium, thereby realize CO
2gas solidifies, and obtains the solution that is rich in potassium ion simultaneously.
The CO of the rich potassium solution of pyroprocess coproduction provided by the invention
2mineralising method, mainly comprises following processing step:
(1) mineral dust that is rich in potassium felspar sand of pulverizing is fully mixed with calcium chloride, at the temperature that is not less than 600 ℃, carry out conversion reaction; Conventionally at the temperature of 600 ~ 1000 ℃, carry out;
(2) material after abundant step (1) conversion reaction is placed in to reactor and adds water, pass into CO
2, at CO
2dividing potential drop is 0.3 ~ 15MPa, and temperature is mineralising reaction under the condition of 50 ~ 350 ℃;
(3) abundant step (2) the reacted feed liquid of mineralising 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 containing mineralization product calcium carbonate.
In technique scheme of the present invention, in step (1), be rich in the mineralising powder of potassium felspar sand and the proportioning of calcium chloride can be determined by the stoichiometry of chemical reaction.Being rich in the mineralising powder of potassium felspar sand and the mass ratio of calcium chloride generally can be in 0.3 ~ 2 scope.
In technique scheme of the present invention, the conversion reaction time in step (1) has a certain impact to the conversion of potassium felspar sand.Being rich in the mineral dust of potassium felspar sand and the conversion reaction time of calcium chloride is not less than 10min conventionally, generally in the scope of 10 ~ 200min.
In technique scheme of the present invention, the not strict restriction of the add-on of water in step (2), as long as the feed liquid that the material after itself and conversion reaction is made into can make and CO
2mineralising reaction successfully carry out all can.Mass ratio between 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 step (2), the reaction times has a certain impact to mineralising efficiency.Material after conversion reaction and CO
2the mineralising reaction times is not less than 10min conventionally, generally in 10 ~ 200min scope.
In technique scheme of the present invention, for reaction can be carried out better, the reaction in step (2) is preferably carried out under the condition that has stirring, and its stir speed (S.S.) can be 50 ~ 1500r/min.
In technique scheme of the present invention, described in be rich in potassium felspar sand mineral dust preferentially adopt potassium mass content with K
2o meter is not less than 5% mineral dust.In mineral dust, potassium-bearing mineral composition comprises at least one in potash feldspar, sanidine and microline.
In technique scheme of the present invention, in order to make conversion reaction and mineralising reaction, particularly conversion reaction can be carried out better, and mineral dust particle size is preferably not more than 50 orders.
The CO of the rich potassium solution of pyroprocess coproduction provided by the invention
2mineralising method, by CO
2mineralisation process completes in two steps, first make the mineral dust that is rich in potassium felspar sand fully mix with calcium chloride, under the high temperature that is not less than 600 ℃, between solid phase, carry out conversion reaction, destroy the stable crystalline structure of potassium felspar sand, generate active alkaline silicoaluminate calcium salt, then the material after conversion reaction is added water and passes into CO
2carry out mineralising reaction, by CO
2mineralising is stable solid carbonic acid calcium, thereby realizes CO
2gas mineralising, potassium ion enters liquid phase simultaneously, obtains being rich in the rich potassium solution of potassium ion.Method of the present invention, the conversion reaction of the mineral dust that is rich in potassium felspar sand under calcium chloride effect, at high temperature carry out, because high temperature can be broken the stable molecular structure of potassium felspar sand, be conducive to reacting between itself and calcium chloride, potassium component is separated out, therefore greatly improved the transformation efficiency of potassium felspar sand, in ore, the transformation efficiency of potassium felspar sand component can be up to 96%, the CO of the rich potassium solution of the coproduction that is 201110382112.4 at the application number of front proposition than applicant
2mineralising method peak rate of conversion 13%, has improved 6.3 times, and potassium felspar sand utilization ratio improves greatly.Again due to be rich in the mineral dust of potassium felspar sand and calcium chloride at high temperature resultant of reaction be active alkaline silicoaluminate calcium salt, by active alkaline silicoaluminate calcium salt and CO
2gas carries out mineralising reaction, directly passes into CO than the ore powder that is rich in potassium felspar sand is joined to calcium chloride solution
2gas carries out mineralising reaction, has obviously improved CO
2the mineralising efficiency of gas.
The CO of the rich potassium solution of pyroprocess coproduction of the present invention
2mineralising method is implemented, and not only can realize CO
2mineralising, make CO
2become stable calcium carbonate solid from gaseous state, also realized the extraction of potassium element in insoluble potassium ore stone simultaneously, produce sufficient potassium resource is provided for potash fertilizer.
The present invention is in other mineralising methods, easy to operate and safe, equipment requirements is low, it is simple to control parameter, and production technique is simple, mineralising efficiency 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, equipment and technology require low, easily realize industrial production.
Accompanying drawing explanation:
Accompanying drawing 1 is the technical process schematic block diagram of one embodiment of the invention.
In the accompanying drawings, 1 is ore grinding equipment; 2 is conversion reaction equipment; The 3rd, CO
2mineralising conversion unit; The 4th, solid-liquid separating equipment.
Embodiment
To closing embodiment, the present invention is specifically described below, so that personnel's the understanding of the present invention of affiliated technical field.What be necessary to particularly point out at this is; embodiment is just for the present invention will be further described; can not be interpreted as limiting the scope of the invention; affiliated art skilled person; according to the invention described above content, the present invention is made improvement and the adjustment of non-intrinsically safe, should still belong to protection scope of the present invention.
By the potassium felspar sand of exploiting out, carry out fragmentation, ball milling, makes its particle size be less than 200 orders.The potassium felspar sand powder of 2.5g is inserted to porcelain boat with the calcium chloride powder of 2.5g fully to be mixed, porcelain boat is put into tubular react furnace, be warming up to 800 ℃, while naturally cooling to 80 ℃ after reaction 60min, take out porcelain boat, material after conversion reaction is taken out, add the water of 75ml to be placed in reactor, be warming up to 150 ℃, pass into CO
2gas boosts to 4MPa, and stir speed (S.S.) is 250r/min, after reaction 120min, stops stirring.Question response still is cooled to 80 ℃ of left and right, and pressure release to normal pressure is opened reactor, and feed liquid after mineralising reaction is filtered, and obtains containing CaCO
3solid phase, liquid phase is the rich potassium solution that is rich in potassium ion.In the present embodiment ore, the transformation efficiency of potassium felspar sand component is 84.5%.
By the potassium felspar sand of exploiting out, carry out fragmentation, ball milling, makes its particle size be less than 325 orders.2.5g potassium felspar sand is inserted to porcelain boat with 5g calcium chloride powder fully to be mixed, porcelain boat is put into tubular react furnace and be warming up to 950 ℃, while naturally cooling to 80 ℃ after reaction 30min, take out porcelain boat, material after conversion reaction is taken out, add the water of 75ml to be placed in reactor, be warming up to 150 ℃, pass into CO
2gas boosts to 4MPa, and stir speed (S.S.) is 250r/min, after reaction 120min, stops stirring.Question response still is cooled to 80 ℃ of left and right, and pressure release to normal pressure is opened reactor, and feed liquid after mineralising reaction is filtered, and obtains containing CaCO
3solid phase, liquid phase is the rich potassium solution that is rich in potassium ion.In the present embodiment ore, the transformation efficiency of potassium felspar sand component is 96%
By the potassium felspar sand of exploiting out, carry out fragmentation, ball milling, makes its particle size be less than 325 orders.2.5g potassium felspar sand is inserted to porcelain boat with 1g calcium chloride powder fully to be mixed, porcelain boat is put into tubular react furnace and be warming up to 600 ℃, while naturally cooling to 80 ℃ after reaction 60min, take out porcelain boat, material after conversion reaction is taken out, add 25ml pure water to be placed in reactor, be warming up to 100 ℃, pass into CO
2pressure rises to 2MPa.Stir speed (S.S.) is 250r/min, after reaction 120min, stops stirring.Question response still is cooled to 80 ℃ of left and right, and pressure release to normal pressure is opened reactor, and feed liquid after mineralising reaction is filtered, and obtains containing CaCO
3solid phase, liquid phase is the rich potassium solution that is rich in potassium ion.In the present embodiment ore, the transformation efficiency of potassium felspar sand component is 45%
Embodiment 4:
By the potassium felspar sand of exploiting out, carry out fragmentation, ball milling, makes its particle size be less than 150 orders.2.5g potassium felspar sand is inserted to porcelain boat with 6g calcium chloride powder fully to be mixed, porcelain boat is put into tubular react furnace and be warming up to 900 ℃, while naturally cooling to 80 ℃ after reaction 30min, take out porcelain boat, material after conversion reaction is taken out, add the water of 75ml to be placed in reactor, be warming up to 150 ℃, pass into 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 question response still is cooled to 80 ℃ of left and right, and pressure release to normal pressure is opened reactor, and feed liquid after mineralising reaction is filtered, and obtains containing CaCO
3solid phase, liquid phase is the rich potassium solution that is rich in potassium ion.In the present embodiment ore, the transformation efficiency of potassium felspar sand component is 65%.
Claims (5)
1. the CO of the rich potassium solution of pyroprocess coproduction
2mineralising method, is characterized in that mainly comprising following processing step:
(1) by the mineral dust that is rich in potassium felspar sand of pulverizing and calcium chloride 0.3～2 ratio batching in mass ratio, after fully mixing, be no less than 10min in being not less than conversion reaction at 600 ℃ of temperature;
(2) material after abundant step (1) conversion reaction is placed in to reactor and adds water, pass into CO
2, at CO
2dividing potential drop is 0.3～15MPa, and temperature is 50～350 ℃, and under the condition that stir speed (S.S.) is 50～1500r/min, mineralising reaction is no less than 10min, and wherein the mass ratio of the inventory after add-on and the conversion reaction of water is 1～100;
(3) abundant step (2) the reacted feed liquid of mineralising 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 calcium carbonate.
2. the CO of the rich potassium solution of a kind of pyroprocess coproduction according to claim 1
2mineralising method, is characterized in that, the conversion reaction temperature of step (1) is 600～1000 ℃.
3. the CO of the rich potassium solution of pyroprocess coproduction according to claim 1 and 2
2mineralising method, is characterized in that, described in be rich in the mineral dust potassium mass content of potassium felspar sand, with K
2o meter is not less than 5%.
4. the CO of the rich potassium solution of pyroprocess coproduction according to claim 3
2mineralising method, is characterized in that, described in be rich in potassium felspar sand mineral dust mineralogical composition comprise at least one in potash feldspar, sanidine and microline.
5. the CO of the rich potassium solution of pyroprocess coproduction according to claim 4
2mineralising 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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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102491795B (en) * | 2011-11-25 | 2013-02-27 | 四川大学 | CO2 mineralization method for co-producing potassium-rich solution |
| CN102899679B (en) * | 2012-10-24 | 2015-08-19 | 四川大学 | Utilize gypsum mineralising CO 2the method of co-producing sulfuric acid |
| CN103466661B (en) * | 2013-08-08 | 2017-08-15 | 四川大学 | One kind utilizes potassium feldspar calcium sulfate mineralising CO2The method of co-producing sulfuric acid potassium |
| 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 |
| CN109133076B (en) * | 2018-08-31 | 2020-06-30 | 贺州市骏鑫矿产品有限责任公司 | Potash feldspar iron removal process method |
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| CN101134680A (en) * | 2007-07-31 | 2008-03-05 | 合肥工业大学 | Method for extracting active potassium from potash feldspar under normal pressure |
| CN101831561A (en) * | 2010-04-23 | 2010-09-15 | 华东理工大学 | Method for decomposing potassium feldspar to extract soluble potassium |
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|---|---|---|---|---|
| CN101134680A (en) * | 2007-07-31 | 2008-03-05 | 合肥工业大学 | Method for extracting active potassium from potash feldspar under normal pressure |
| CN101831561A (en) * | 2010-04-23 | 2010-09-15 | 华东理工大学 | Method for decomposing potassium feldspar to extract soluble potassium |
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| 周蔚 等.青海省非可溶性钾矿提钾工艺初步研究.《青海大学学报（自然科学版）》.2010,第28卷(第5期),27-29、41. * |
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