CN103693659A - Method for concurrent production of potassium chloride and mineralization fixation of CO2 - Google Patents
Method for concurrent production of potassium chloride and mineralization fixation of CO2 Download PDFInfo
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- CN103693659A CN103693659A CN201310558115.8A CN201310558115A CN103693659A CN 103693659 A CN103693659 A CN 103693659A CN 201310558115 A CN201310558115 A CN 201310558115A CN 103693659 A CN103693659 A CN 103693659A
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Abstract
The invention belongs to the comprehensive field of potassium fertilizer production and CO2 emission reduction, and provides a method for concurrent production of potassium chloride and mineralization fixation of CO2. The process steps comprise: (1) adopting potassium feldspar, calcium chloride and coal as raw materials, preparing materials, carrying out ball milling, and carrying out pressing molding or pelletizing; (2) conveying the molded material or the material balls into a rotary kiln from the kiln tail, conveying air into the rotary kiln from the kiln head, and controlling a residence time of the molded material or the material balls at a temperature range of 800-1000 DEG C to 20-40 min; (3) crushing the calcinated material, and adding water to carry out potassium leaching through the water; (4) adding water to the potassium leaching residue to carry out pulp conditioning, and introducing CO2 to carry out a mineralization reaction; (5) carrying out returning of the potassium leaching solution so as to be used for leaching of potassium from the calcinated material when the Baume degree of the potassium leaching solution is less than or equal to 29, and carrying out evaporation concentration on the potassium leaching solution to achieve the Baume degree of 42-42.5 when the Baume degree of the potassium leaching solution is more than 29, and cooling to carry out potassium chloride crystallization; and (6) cooling the potassium extraction mother liquor to carry out calcium chloride crystallization, and carrying out solid-liquid separation to obtain calcium chloride and the calcium extraction mother liquor.
Description
Technical field
The invention belongs to potash fertilizer produces and CO
2reduce discharging general field, particularly a kind of production Repone K while mineralising fixation of C O
2method.
Background technology
The CO that fossil feedstock burning produces
2discharge is the main factor that causes Global warming, how to reduce CO
2discharge, alleviates Greenhouse effect more effectively, has become countries in the world major issue urgently to be resolved hurrily.At present, process on a large scale CO
2method mainly contain geological storage, seal up for safekeeping ocean and CO
2three kinds of methods of mineralising, research shows, CO
2mineralising is a kind of safe, stable CO
2fixing means, but the main natural crystal of large calcium-magnesium-containing that adopts is such as forsterite, serpentine, wollastonite etc. both at home and abroad, and Industrial Solid Waste is such as slag and phosphogypsum etc., mineralising reaction primary product is calcium carbonate and the magnesiumcarbonate that added value is low, in addition, the common speed of response of these mineralisation process is slow, needs to adopt the high-temperature activation pre-treatment of power consumption to strengthen.Therefore, current CO
2mineralising is sealed up for safekeeping with other mode of sealing up for safekeeping and is compared, and on cost, does not preponderate.How to improve CO
2the economy that mineralising is sealed up for safekeeping is the problem that prior art must solve.
Potash fertilizer is the needed a kind of important fertilizer of agriculture production, countries and regions at water-soluble potassium scarcity of resources, often need to utilize water-insoluble potassium resource to produce potash fertilizer, potassium felspar sand is a kind of water-insoluble potassium resource, but will extract from potassium felspar sand, potassium difficulty is large, cost is high, numerous research institutions and enterprise have carried out a large amount of research and experiments around carry potassium from potassium felspar sand, and attempt just potash fertilizer and produce and CO
2mineralising is sealed up for safekeeping and is combined, and improves economy.CN102701253A discloses the CO of the rich potassium solution of a kind of pyroprocess coproduction
2mineralising method, first the method is carried out pyrolytic conversion by potassium felspar sand powder and calcium chloride powder and is reacted, and then under pressurization and comparatively high temps, carries out flooding potassium and CO simultaneously
2mineralising obtains rich potassium solution and mineralization product.Although the method has realized CO
2mineralising and the combination of carrying potassium from potassium felspar sand, but be difficult to carry out suitability for industrialized production, reason is: (1) potassium felspar sand all carries out pyrolytic conversion with the heap powder that falls apart with calcium chloride and reacts, loose heap material is easily emanated in moving process, because calcium chloride fusing point is only～780 ℃, when conversion reaction temperature surpasses its fusing point, calcium chloride will melt, and causes ring formation in reactor and is difficult to long-period stable operation; (2) because potassium felspar sand reacts with the pyrolytic conversion of calcium chloride, be thermo-negative reaction, need outside heat supply, and conversion reaction in the method is carried out in tubular react furnace, relies on electric energy that reaction institute heat requirement is provided, and causes high cost; (3) carry out flooding potassium and CO simultaneously
2mineralising, owing to containing a large amount of chlorions in flooding potassium solution, this flooding potassium and CO in addition
2mineralisation process is at 50～350 ℃, CO
2dividing potential drop is to carry out under the condition of 0.3～15MPa, causes chlorion serious to equipment corrosion, and cost of equipment drops into too high.
Summary of the invention
The object of the invention is to overcome the deficiency that prior art exists, a kind of production Repone K mineralising fixation of C O is simultaneously provided
2method, to solve ring formation in reactor, mineralising conversion unit material is required to problem high and that thermal source cost is high, promote suitability for industrialized production.
Production Repone K of the present invention is mineralising fixation of C O simultaneously
2method, processing step is as follows:
(1) take potassium felspar sand particle, calcium chloride particle and coal particle is raw material, according to potassium felspar sand butt quality: calcium chloride butt quality: (0.6～1.5) ︰'s coal butt quality=1 ︰ (0.1～0.25) prepares burden, add the ball mill with drying installation to be milled to particle diameter≤0.15mm the solid mixture of described composition, then the mixed powder after ball milling is added to binding agent and mix after be pressed into moulding mixture, or the mixed powder after ball milling is added to binding agent and water and mix after be prepared into pellet, pellet is standby after drying;
(2) moulding mixture of being prepared by step (1) or pellet are sent into rotary kiln from the kiln tail of rotary kiln, air is sent into rotary kiln from the kiln hood of rotary kiln, in rotary kiln, air and moulding mixture or pellet countercurrent movement, the contained coal combustion of moulding mixture in motion or pellet produces high temperature, described moulding mixture or pellet are 20～40min 800～1000 ℃ of interval residence time, the high-temperature flue gas producing in moulding mixture or pellet roasting process leaves rotary kiln after kiln tail and the pellet that enters or moulding mixture heat exchange, after the roasting material that moves to kiln hood and the air heat-exchange entering, leaves rotary kiln;
(3) step (2) gained roasting material is pulverized, then added water under agitation in normal pressure, 20～50 ℃ of flooding potassium, after soaking potassium and completing, carry out solid-liquid separation and obtain soaking potassium liquid and soak potassium slag; The liquid-solid ratio that potassium process is soaked in control for (2～5) ︰ 1, wherein, the measure unit of solid phase quality be kilogram, the measure unit of liquid phase volume for liter;
(4) the potassium slag that soaks step (3) being obtained adds water and sizes mixing, and then gained slurry is added to mineralising reactor and passes into CO
2carry out mineralising reaction, CO
2pressure be controlled at 0.2～1MPa, mineralising temperature of reaction is 50～150 ℃, has reacted rear solid-liquid separation and has obtained mineralising slag and mineralising mother liquor; The liquid-solid ratio of controlling slurry be (3～6) ︰ 1, wherein, the measure unit of solid phase quality be kilogram, the measure unit of liquid phase volume is liter;
(5) during the degree Beaume that soaks potassium liquid obtaining when step (3) (° B é)≤29, returned to the leaching for roasting material potassium, when the degree Beaume that soaks potassium liquid (° B é) > 29 that step (3) obtains, by its evaporation concentration to degree Beaume, be 42～42.5, then be cooled to 80～85 ℃ and carry out Repone K crystallization, after crystallization completes, solid-liquid separation obtains Repone K and carries potassium mother liquor;
(6) step (5) gained is carried to potassium mother liquor and be cooled to 25～40 ℃ and carry out crystallization of calcium chloride, after crystallization completes, solid-liquid separation obtains calcium chloride and carries mother liquor of calcium.
In aforesaid method, binding agent add-on when step (1) is prepared moulding mixture is 1.5～5% of three kinds of total butt quality of raw material, and the moulding mixture of preparation can be the shapes such as column, sheet; Binding agent add-on when step (1) is prepared pellet is 1.5～5% of three kinds of total butt quality of raw material, water add-on is 10～13% of three kinds of total butt quality of raw material, the diameter of prepared pellet is 5～15mm, and the dry temperature of pellet is at least 150 ℃, is at least 15min time of drying.
In aforesaid method, the described binding agent of step (1) is pitch, sodium humate, water glass or wilkinite.
In aforesaid method, the time of the described flooding potassium of step (3) is 10～50min, and the time of the described mineralising reaction of step (4) is 20～60min.
In aforesaid method, in step (5), Repone K crystallization time is 1～2h, and in step (6), the crystallization of calcium chloride time is 3～4h.
In aforesaid method, the particle diameter≤2mm of described raw material potassium felspar sand particle, calcium chloride particle and coal particle, roasting material is crushed to≤1mm in step (3).
In aforesaid method, by described mineralising mother liquor for soaking sizing mixing of potassium slag, by the described mother liquor of calcium of carrying for the leaching of roasting material potassium, by step (6) gained calcium chloride for the preparation of moulding mixture or pellet.
In aforesaid method, described moulding mixture or pellet are to control by adjusting pitch angle and the rotating speed of rotary kiln 800～1000 ℃ of interval residence time.
In aforesaid method, rotary kiln is lighted a fire by passing into Sweet natural gas or spraying into coal dust when starting.
The present invention has following beneficial effect:
1, the method for the invention is made moulding mixture or pellet by potassium felspar sand and calcium chloride raw material, in batching, added coal simultaneously, by the ash fusion point of reaction mass integral body be increased to 1050 ℃ and more than, fusing point far above calcium chloride, this can have been avoided the problem that in the kiln in pyrolytic conversion reaction, ring formation causes rotary kiln to stop up, on the other hand, so that pyrolytic conversion reaction institute heat requirement to be provided than more cheap coals such as electricity, Sweet natural gas or liquid fuels, reduced significantly cost.
Gu 2, potassium felspar sand is consolidate-heterogeneous reaction of high temperature with reacting of calcium chloride, solid reactant is prepared into moulding mixture to the method for the invention or pellet is conducive to fully contact between each reactant composition, the speed that can add fast response, in 20～40min, the transformation efficiency of Potassium in K Feldspar reaches as high as 98%(and sees embodiment 3), improved the economy of conversion reaction process.
3, the method for the invention is first carried out the leaching of potassium under normal pressure, lesser temps, then carries out CO
2mineralising, because the operation of flooding potassium can fully remove soluble chloride in roasting material, thereby avoided high-concentration chlorine ion corrosion to mineralizing device under High Temperature High Pressure, thus can reduce the requirement to mineralising and subsequent process equipment material, can reduce the input of cost of equipment.
4, the present invention also provides the method for separated Repone K and calcium chloride from soak potassium liquid, this has obtained the chemical fertilizer Repone K (quality meets GB6549-2011) of China's agriculture production famine on the one hand, simultaneously, isolated calcium chloride can recycle, reduce the consumption of calcium chloride, improved significantly the economy of process.
5, the method for the invention is carried out the conversion reaction of potassium felspar sand in rotary kiln, and technique is easy to amplify and realizes suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the first process flow sheet of the method for the invention.
Fig. 2 is the second process flow sheet of the method for the invention.
Embodiment
By the following examples to production Repone K while mineralising fixation of C O of the present invention
2method be described further, in following each embodiment, the chemical constitution of three kinds of raw materials is calculated in mass percent and is respectively: potassium felspar sand, K
2o11%, Al
2o
316.4%, SiO
260.2%; Calcium chloride, CaCl
295.3%; Coal, fixed carbon 77.9%.The vertical ball mill adopting in following each embodiment is with drying installation, and by Wuhan, mine locating machine works produces, and model is XMQ-Φ 240 * 90A, also can adopt other commercially available ball mills with drying installation.
Embodiment 1
As shown in Figure 1, processing step is as follows for the process flow sheet of the present embodiment:
(1) respectively by potassium felspar sand, calcium chloride and coal pulverizer are to particle diameter≤2mm, according to potassium felspar sand butt quality: calcium chloride butt quality: coal butt quality=1 ︰ 1 ︰ 0.14 prepares burden, the solid mixture of described composition is added and in vertical ball mill, is milled to particle diameter≤0.10mm, then after the mixed powder after ball milling being added to the sodium humate of three kinds of total butt quality 1.5% of raw material and the water of three kinds of total butt quality 13% of raw material and mixing, adopt ordinary method (as disk pelletizing method, cylinder pelletizing method) be prepared into the pellet that diameter is 5～8mm, pellet is standby after 260 ℃ of dry at least 15min, the ash fusion point of the dry pellet of gained is 1150 ℃.
(2) pellet of being prepared by step (1) is sent into rotary kiln continuously from the kiln tail of rotary kiln, air is sent into rotary kiln continuously from the kiln hood of rotary kiln, in rotary kiln, air and pellet countercurrent movement, the contained coal combustion of pellet in motion produces high temperature, described pellet is 40min 800～900 ℃ of interval residence time, the high-temperature flue gas producing in pellet roasting process leaves rotary kiln after kiln tail and the pellet heat exchange that enters, after the roasting material that moves to kiln hood and the air heat-exchange entering, leaves rotary kiln; Described rotary kiln is of a size of Φ 200 * 2000mm, and obliquity is 4%, and the rotating speed of controlling rotary kiln is 3.5r/min.
(3) step (2) gained roasting material is crushed to particle diameter≤0.15mm, then adds water, flooding potassium 10min under normal pressure, 50 ℃ and agitation condition, soaks after potassium completes and filters and obtain soaking potassium liquid and soak potassium slag; The liquid-solid ratio that potassium process is soaked in control is 3 ︰ 1, and wherein, the measure unit of solid phase quality is kilogram that the measure unit of liquid phase volume is for rising.
(4) the potassium slag that soaks step (3) being obtained adds adjusting slurry and sizes mixing, the add-on of described adjusting slurry is that to make the liquid-solid ratio of slurry be 3 ︰ 1, in slurry, the measure unit of solid phase quality is kilogram, and the measure unit of liquid phase volume, for rising, then adds described slurry mineralising reactor and passes into CO
2carry out mineralising reaction, CO
2pressure be controlled at 0.2MPa, mineralising temperature of reaction is 100 ℃, the mineralising reaction times is 30min, filters to obtain mineralising slag and mineralising mother liquor after having reacted; Described adjusting slurry is solid-liquid separation gained mineralising mother liquor after mineralising reaction, insufficient section make up water.
(5) when step (3) obtain soak degree Beaume≤29 of potassium liquid time, returned to flooding potassium operation for the leaching of roasting material potassium, when step (3) obtain soak the degree Beaume > 29 of potassium liquid time, analyzing gained soaks the concentration of Repone K and calcium chloride in potassium liquid and is respectively 14.6wt% and 33.6wt%, by its evaporation concentration to degree Beaume, be 42, be then cooled to 80 ℃ and carry out Repone K crystallization, crystallization time is 1h, after crystallization completes, filter to obtain Repone K and carry potassium mother liquor; The concentration of the above-mentioned Repone K of every 1000mL and calcium chloride is respectively the potassium liquid that soaks of 14.6wt% and 33.6wt%, and can to obtain KCl content be 90% 91 grams of Potassium Chloride Products (base of giving money as a gift).
(6) step (5) gained being carried to potassium mother liquor is cooled to 40 ℃ and carries out crystallization of calcium chloride, crystallization time is 4h, after crystallization completes, filter to obtain calcium chloride and carry mother liquor of calcium, by carrying mother liquor of calcium, be back to flooding potassium operation for the leaching of roasting material potassium, calcium chloride be circulated to the burden process of step (1); The concentration of the above-mentioned Repone K of every 1000mL and calcium chloride is respectively soaking potassium liquid and can obtaining CaCl of 14.6wt% and 33.6wt%
2content is 93% 209 grams of calcium chloride products (base of giving money as a gift).
In the present embodiment, CO
2mineralization rate be 9%(kilogram of CO
2/ kilogram potassium felspar sand), the transformation efficiency of Potassium in K Feldspar is 86%.
Embodiment 2
As shown in Figure 2, processing step is as follows for the process flow sheet of the present embodiment:
(1) respectively by potassium felspar sand, calcium chloride and coal pulverizer to particle diameter≤2mm, according to potassium felspar sand butt quality: calcium chloride butt quality: coal butt quality=1 ︰ 0.6 ︰ 0.1 prepares burden, the solid mixture of described composition is added and in vertical ball mill, is milled to particle diameter≤0.075mm, then the mixed powder after ball milling is added to pitch or the water glass of three kinds of total butt quality 3% of raw material and mix after be pressed into the moulding mixture that is of a size of Φ 10*5mm, the ash fusion point of gained moulding mixture is 1180 ℃.
(2) moulding mixture of being prepared by step (1) is sent into rotary kiln continuously from the kiln tail of rotary kiln, air is sent into rotary kiln continuously from the kiln hood of rotary kiln, in rotary kiln, air and moulding mixture countercurrent movement, the contained coal combustion of moulding mixture in motion produces high temperature, described moulding mixture is 40min 800～900 ℃ of interval residence time, the high-temperature flue gas producing in moulding mixture roasting process leaves rotary kiln after kiln tail and the moulding mixture heat exchange that enters, after the roasting material that moves to kiln hood and the air heat-exchange entering, leaves rotary kiln; Described rotary kiln is of a size of Φ 200 * 2000mm, and obliquity is 3%, and the rotating speed of controlling rotary kiln is 4r/min.
(3) step (2) gained roasting material is crushed to particle diameter≤1mm, then adds water, flooding potassium 10min under normal pressure, 50 ℃ and agitation condition, soaks after potassium completes and filters and obtain soaking potassium liquid and soak potassium slag; The liquid-solid ratio that potassium process is soaked in control is 2 ︰ 1, and wherein, the measure unit of solid phase quality is kilogram that the measure unit of liquid phase volume is for rising.
(4) the potassium slag that soaks step (3) being obtained adds adjusting slurry and sizes mixing, the add-on of described adjusting slurry is that to make the liquid-solid ratio of slurry be 3 ︰ 1, in slurry, the measure unit of solid phase quality is kilogram, and the measure unit of liquid phase volume, for rising, then adds described slurry mineralising reactor and passes into CO
2carry out mineralising reaction, CO
2pressure be controlled at 1MPa, mineralising temperature of reaction is 50 ℃, the mineralising reaction times is 60min, filters to obtain mineralising slag and mineralising mother liquor after having reacted; Described adjusting slurry is solid-liquid separation gained mineralising mother liquor after mineralising reaction, insufficient section make up water.
(5) when step (3) obtain soak degree Beaume≤29 of potassium liquid time, returned to flooding potassium operation for the leaching of roasting material potassium, when step (3) obtain soak the degree Beaume > 29 of potassium liquid time, analyzing gained soaks the concentration of Repone K and calcium chloride in potassium liquid and is respectively 17.8wt% and 30.2wt%, by its evaporation concentration to degree Beaume, be 42.5, then be cooled to 90 ℃ and carry out Repone K crystallization, crystallization time is 2h, after crystallization completes, filter to obtain Repone K and carry potassium mother liquor; The concentration of the above-mentioned Repone K of every 1000mL and calcium chloride is respectively the potassium liquid that soaks of 17.8wt% and 30.2wt%, and can to obtain KCl content be 91% 111 grams of Potassium Chloride Products (base of giving money as a gift).
(6) step (5) gained being carried to potassium mother liquor is cooled to 25 ℃ and carries out crystallization of calcium chloride, crystallization time is 3h, after crystallization completes, filter to obtain calcium chloride and carry mother liquor of calcium, by carrying mother liquor of calcium, be back to flooding potassium operation for the leaching of roasting material potassium, calcium chloride be circulated to the burden process of step (1); The concentration of the above-mentioned Repone K of every 1L and calcium chloride is respectively soaking potassium liquid and can obtaining CaCl of 17.8wt% and 30.2wt%
2content is 94% 186 grams of calcium chloride products (base of giving money as a gift).
In the present embodiment, CO
2mineralization rate be 7%(kilogram of CO
2/ kilogram potassium felspar sand), the transformation efficiency of Potassium in K Feldspar is 61%.
Embodiment 3
As shown in Figure 1, processing step is as follows for the process flow sheet of the present embodiment:
(1) respectively by potassium felspar sand, calcium chloride and coal pulverizer are to particle diameter≤2mm, according to potassium felspar sand butt quality: calcium chloride butt quality: coal butt quality=1 ︰ 1.5 ︰ 0.25 prepare burden, the solid mixture of described composition is added and in vertical ball mill, is milled to particle diameter≤0.10mm, then after the mixed powder after ball milling being added to the wilkinite of three kinds of total butt quality 5% of raw material and the water of three kinds of total butt quality 10% of raw material and mixing, adopt ordinary method (as disk pelletizing method, cylinder pelletizing method) be prepared into the pellet that diameter is 10～15mm, pellet is standby after 150 ℃ of dry at least 30min, the ash fusion point of the dry pellet of gained is 1060 ℃.
(2) pellet of being prepared by step (1) is sent into rotary kiln continuously from the kiln tail of rotary kiln, air is sent into rotary kiln continuously from the kiln hood of rotary kiln, in rotary kiln, air and pellet countercurrent movement, the contained coal combustion of pellet in motion produces high temperature, described pellet is 20min 900～1000 ℃ of interval residence time, the high-temperature flue gas producing in pellet roasting process leaves rotary kiln after kiln tail and the pellet heat exchange that enters, after the roasting material that moves to kiln hood and the air heat-exchange entering, leaves rotary kiln; Described rotary kiln is of a size of Φ 200 * 2000mm, and obliquity is 3.5%, and the rotating speed of controlling rotary kiln is 3r/min.
(3) step (2) gained roasting material is crushed to particle diameter≤0.15mm, then adds water, flooding potassium 50min under normal pressure, 20 ℃ and agitation condition, soaks after potassium completes and filters and obtain soaking potassium liquid and soak potassium slag; The liquid-solid ratio that potassium process is soaked in control is 5 ︰ 1, and wherein, the measure unit of solid phase quality is kilogram that the measure unit of liquid phase volume is for rising.
(4) the potassium slag that soaks step (3) being obtained adds adjusting slurry and sizes mixing, the add-on of described adjusting slurry is that to make the liquid-solid ratio of slurry be 6 ︰ 1, in slurry, the measure unit of solid phase quality is kilogram, and the measure unit of liquid phase volume, for rising, then adds described slurry mineralising reactor and passes into CO
2carry out mineralising reaction, CO
2pressure be controlled at 0.2MPa, mineralising temperature of reaction is 150 ℃, the mineralising reaction times is 20min, filters to obtain mineralising slag and mineralising mother liquor after having reacted; Described adjusting slurry is solid-liquid separation gained mineralising mother liquor after mineralising reaction, insufficient section make up water.
(5) when step (3) obtain soak degree Beaume≤29 of potassium liquid time, returned to flooding potassium operation for the leaching of roasting material potassium, when step (3) obtain soak the degree Beaume > 29 of potassium liquid time, analyzing gained soaks the concentration of Repone K and calcium chloride in potassium liquid and is respectively 11.1wt% and 36.8wt%, by its evaporation concentration to degree Beaume, be 42, be then cooled to 85 ℃ and carry out Repone K crystallization, crystallization time is 1h, after crystallization completes, filter to obtain Repone K and carry potassium mother liquor; The concentration of the above-mentioned Repone K of every 1L and calcium chloride is respectively the potassium liquid that soaks of 11.1wt% and 36.8wt%, and can to obtain KCl content be 88% 69 grams of Potassium Chloride Products (base of giving money as a gift).
(6) step (5) gained being carried to potassium mother liquor is cooled to 35 ℃ and carries out crystallization of calcium chloride, crystallization time is 4h, after crystallization completes, filter to obtain calcium chloride and carry mother liquor of calcium, by carrying mother liquor of calcium, be back to flooding potassium operation for the leaching of roasting material potassium, calcium chloride be circulated to the burden process of step (1); The concentration of the above-mentioned Repone K of every 1L and calcium chloride is respectively soaking potassium liquid and can obtaining CaCl of 11.1wt% and 36.8wt%
2content is 92% 230 grams of calcium chloride products (base of giving money as a gift).
In the present embodiment, CO
2mineralization rate be 12%(kilogram of CO
2/ kilogram potassium felspar sand), the transformation efficiency of Potassium in K Feldspar is 98%.
Claims (10)
1. produce Repone K mineralising fixation of C O simultaneously for one kind
2method, it is characterized in that processing step is as follows:
(1) take potassium felspar sand particle, calcium chloride particle and coal particle is raw material, according to potassium felspar sand butt quality: calcium chloride butt quality: (0.6～1.5) ︰'s coal butt quality=1 ︰ (0.1～0.25) prepares burden, add the ball mill with drying installation to be milled to particle diameter≤0.15mm the solid mixture of described composition, then the mixed powder after ball milling is added to binding agent and mix after be pressed into moulding mixture, or the mixed powder after ball milling is added to binding agent and water and mix after be prepared into pellet, pellet is standby after drying;
(2) moulding mixture of being prepared by step (1) or pellet are sent into rotary kiln from the kiln tail of rotary kiln, air is sent into rotary kiln from the kiln hood of rotary kiln, in rotary kiln, air and moulding mixture or pellet countercurrent movement, the contained coal combustion of moulding mixture in motion or pellet produces high temperature, described moulding mixture or pellet are 20～40min 800～1000 ℃ of interval residence time, the high-temperature flue gas producing in moulding mixture or pellet roasting process leaves rotary kiln after kiln tail and the pellet that enters or moulding mixture heat exchange, after the roasting material that moves to kiln hood and the air heat-exchange entering, leaves rotary kiln;
(3) step (2) gained roasting material is pulverized, then added water under agitation in normal pressure, 20～50 ℃ of flooding potassium, after soaking potassium and completing, carry out solid-liquid separation and obtain soaking potassium liquid and soak potassium slag; The liquid-solid ratio that potassium process is soaked in control for (2～5) ︰ 1, wherein, the measure unit of solid phase quality be kilogram, the measure unit of liquid phase volume for liter;
(4) the potassium slag that soaks step (3) being obtained adds water and sizes mixing, and then gained slurry is added to mineralising reactor and passes into CO
2carry out mineralising reaction, CO
2pressure be controlled at 0.2～1MPa, mineralising temperature of reaction is 50～150 ℃, has reacted rear solid-liquid separation and has obtained mineralising slag and mineralising mother liquor; The liquid-solid ratio of controlling slurry be (3～6) ︰ 1, wherein, the measure unit of solid phase quality be kilogram, the measure unit of liquid phase volume is liter;
(5) when step (3) obtain soak degree Beaume≤29 of potassium liquid time, returned to the leaching for roasting material potassium, when step (3) obtain soak the degree Beaume > 29 of potassium liquid time, by its evaporation concentration to degree Beaume, be 42～42.5, then be cooled to 80～85 ℃ and carry out Repone K crystallization, after crystallization completes, solid-liquid separation obtains Repone K and carries potassium mother liquor;
(6) step (5) gained is carried to potassium mother liquor and be cooled to 25～40 ℃ and carry out crystallization of calcium chloride, after crystallization completes, solid-liquid separation obtains calcium chloride and carries mother liquor of calcium.
2. produce according to claim 1 Repone K mineralising fixation of C O simultaneously
2method, it is characterized in that in step (1), the binding agent add-on while preparing moulding mixture is 1.5～5% of three kinds of total butt quality of raw material; Binding agent add-on while preparing pellet is 1.5～5% of three kinds of total butt quality of raw material, and water add-on is 10～13% of three kinds of total butt quality of raw material.
3. produce according to claim 1 Repone K mineralising fixation of C O simultaneously
2method, it is characterized in that the described binding agent of step (1) is pitch, sodium humate, water glass or wilkinite.
4. according to producing Repone K mineralising fixation of C O simultaneously described in arbitrary claim in claims 1 to 3
2method, it is characterized in that the time of the described flooding potassium of step (3) is 10～50min, the time of the described mineralising of step (4) reaction is 20～60min.
5. according to producing Repone K mineralising fixation of C O simultaneously described in arbitrary claim in claims 1 to 3
2method, it is characterized in that in step (5) that Repone K crystallization time is 1～2h, in step (6), the crystallization of calcium chloride time is 3～4h.
6. produce according to claim 4 Repone K mineralising fixation of C O simultaneously
2method, it is characterized in that in step (5) that Repone K crystallization time is 1～2h, in step (6), the crystallization of calcium chloride time is 3～4h.
7. according to producing Repone K mineralising fixation of C O simultaneously described in arbitrary claim in claims 1 to 3
2method, it is characterized in that the particle diameter≤2mm of described raw material potassium felspar sand particle, calcium chloride particle and coal particle, roasting material is crushed to≤1mm in step (3).
8. produce according to claim 4 Repone K mineralising fixation of C O simultaneously
2method, it is characterized in that the particle diameter≤2mm of described raw material potassium felspar sand particle, calcium chloride particle and coal particle, roasting material is crushed to≤1mm in step (3).
9. produce according to claim 5 Repone K mineralising fixation of C O simultaneously
2method, it is characterized in that the particle diameter≤2mm of described raw material potassium felspar sand particle, calcium chloride particle and coal particle, roasting material is crushed to≤1mm in step (3).
10. according to producing Repone K mineralising fixation of C O simultaneously described in arbitrary claim in claims 1 to 3
2method, it is characterized in that: by described mineralising mother liquor for soaking sizing mixing of potassium slag, by the described mother liquor of calcium of carrying for the leaching of roasting material potassium, by step (6) gained calcium chloride for the preparation of moulding mixture or pellet.
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|---|---|---|---|
| CN201310558115.8A CN103693659B (en) | 2013-11-11 | 2013-11-11 | Method for concurrent production of potassium chloride and mineralization fixation of CO2 |
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| CN106629802A (en) * | 2016-11-21 | 2017-05-10 | 华东理工大学 | Method for mineralizing carbon dioxide by production waste residues in potassium feldspar sub-molten salt method |
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