CN105039744A - Method for preparing solid carbon dioxide and calcium metal through calcite - Google Patents
Method for preparing solid carbon dioxide and calcium metal through calcite Download PDFInfo
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- CN105039744A CN105039744A CN201510447486.8A CN201510447486A CN105039744A CN 105039744 A CN105039744 A CN 105039744A CN 201510447486 A CN201510447486 A CN 201510447486A CN 105039744 A CN105039744 A CN 105039744A
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- carbon dioxide
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- calcite
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- calcium oxide
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Abstract
The invention discloses a method for preparing solid carbon dioxide and calcium metal through calcite. The method comprises the following steps that (1) the calcite is subjected to coarse breaking and fine breaking, so that calcite powder of 1-3 mm is obtained; (2) the calcite powder is placed in a calcinatory to be calcinated, so that calcium oxide and carbon dioxide gas are obtained; (3) the calcium oxide and ferrosilicon powder are mixed, subjected to a vacuum thermal reduction reaction and gasified after reduction, replacement and sublimation, and released calcium steam is collected and cooled to obtain calcium metal solid and a finished calcium silicate product; and the carbon dioxide gas obtained in the step (2) is condensed into liquid carbon dioxide which is further made into the solid carbon dioxide. By means of the method, the problem that lime calcined through the traditional methods is polluted by coal, fuel and other burner gas is solved; in the whole technological process, chlorine is not generated, emission of the three wastes is avoided, and the environment is not polluted; operation is safe and reliable, the obtained calcium metal and dry ice are pre-products for artificially synthesizing hydrocarbon fuel, the market application prospects are wide, and the potential of replacing natural fossil fuel is great.
Description
Technical field
The present invention relates to the preparation method of solidified carbon dioxide and calcium metal, relate to calcite more specifically and prepare solidified carbon dioxide and calcium metal method.
Background technology
Calcium is the metal that we are familiar with very much.Calcium is the element of needed by human.Industrially, the purposes of calcium metal can be used as reductive agent, is used for preparing other metals; As dewatering agent, manufacture raw spirit; In petroleum industry, as sweetening agent; In metallurgical industry, with its deoxidation or desulfuration.The purposes of calcium also has in addition: 1. as the additive of external refining when producing extraordinary quality steel plate in iron and steel metallurgical industry, plays to prevent cast gate from blocking, control inclusion morphology, desulfurization and improve the vital role such as molten steel casting performance; 2. at battery industry for the production of the lead-calcium alloy as lead-acid battery negative pole plate; 3. as the reductive agent of deoxygenation or other chemical compositions in the smelting of non-ferrous metal, rare earth metal and refractory metal; 4. as reductive agent when producing some medicine intermediate in pharmaceutical industries.
The preparation method of calcium has reduction method, electrolytic process, calcium refining three kinds.Reduction method is the main method of producing calcium metal.Usual Wingdale is raw material, through being sintered into calcium oxide, makes reductive agent with aluminium powder.The calcium oxide pulverized mixes by a certain percentage with aluminium powder, and briquetting, reacts under 0.01 vacuum and 1050-1200 DEG C of temperature, generates calcium steam and calcium aluminate, the calcium steam crystallization at 750-400 DEG C restored.Crystalline calcium is melting ingot casting under argon shield again, obtains fine and close calcium ingot.Reduction method produces the rate of recovery of calcium generally about 60%.Electrolysis comparatively is early contact process, and because this method raw material consumption is large, calcium metal solubleness is in the electrolyte high, and current efficiency is low, and poor product quality (chloride about 1%) etc., were improved to the electrolysis of liquid cathode method afterwards.Calcium refining: industrial calcium can obtain high purity calcium through molecular distillation process again.General control distillation temperature is 780-820 DEG C, vacuum tightness 1 × 10
-4.Distillation process is poor to muriate effect in purification calcium, when lower than distillation temperature, can add nitride, make it to form double salt.By adding nitride and vacuum distilling purification, in calcium, the summation of impurity element chlorine, manganese, copper, iron, silicon, aluminium, nickel etc. can drop to 1000-100ppm, obtains the high purity calcium of 99.9%-99.99%.
The method of carbonic acid gas and calcium metal is produced, as neutralization reaction chemical process extract carbon dioxide technology: open Bian ore → coarse crushing → in small, broken bits → abrasive dust → add hydrochloric acid to neutralize → collect carbon dioxide, chemical equation is as follows: CaCO in prior art
3+ 2HCl====CaCl
2+ CO
2↑+H
2o; Decomposition reaction chemical process produces calcium metal, CaCl under the condition of catalyzer
2decompose and obtain calcium metal, chemical equation is as follows: CaCl
2====Ca+Cl
2↑; Roasting method calcium oxide method for making: CaCO
3with coal under the condition of roasting, obtain CaO and CO
2, chemical equation is as follows: CaCO
3+ coal=====CaO+CO
2↑.
The above-mentioned carbonic acid gas mentioned, obtains solidified carbon dioxide by after carbonic acid gas subcooling, and also known as dry ice, its use range is extensive, in food, health, industry, food and drink, have extensive application.Mainly contain: 1. dry ice is in the range of application of food pharmaceutical: successfully can remove the residue of oven for baking, gelatinoid and greasy dirt and the fresh product mixture before not toasting.Effectively settle accounts baking box, mix and blend equipment, conveying belt, moulded product, packaging facilities, grate, stone or metal plate for standing a stove on as a precaution against fire, container, roll shaft, refrigerator inwall, biscuit fire bars etc.The benefit of Dry ice cleaning: the use getting rid of harmful chemical agent, avoids production unit to contact harmful chemicals thing and produces second time rubbish; Draw up or remove the bacterium such as Salmonellas, Li Site bacterium, more thoroughly sterilization, cleaning; Get rid of the damage of water cutter cleaning to electronics; The equipment of minimum degree decomposes; Reduce stoppage time.2. dry ice is in the range of application of industrial mould: tire-mold, rubber mold, urethane mould, polyethylene mould, PET mould, foam mold, injection mold, alloy die-casting, hot core box for casting, cold-box, can remove cotree fat, inefficacy release layer, charing film, greasy dirt, get through venting hole, cleaning rear mold light is as new.On-line cleaning, without the need to cooling and dismounting mould, avoids chemical cleaning method to the corrosion of mould and infringement, mechanical cleaning process to the physical abuse of mould and scuffing, and handling cause degradation shortcoming under mould and die accuracy repeatedly.Crucially, dismounting mould can be exempted and wait for that mould is lowered the temperature these two most time-consuming steps, all like this can reduce stoppage time and be about 80%-95%.Dry ice cleaning benefit: Dry ice cleaning can reduce man-hours in idleness; Reduce structure deteriorate; Extremely effectively clean the equipment of high temperature; Reduce or reduce the use of solvent; Improve the safety of staff; Promote maintenance efficiency; Reduce the production shut-down period, reduce costs, enhance productivity.3. dry ice is in the range of application of entertainment field: be widely used in the making such as stage, arenas, video display, wedding celebration, celebration, party effect and put cigarette, the partial programme dry ice as National Theatre makes effect.
Retrieve the following preparation method about dry ice and calcium metal:
Chinese patent, title:
"herba Eichhorniae is utilized to prepare the method for bio-natural gas and biological dry ice
"; Application Number (patent): CN201110148614.0; Applicant: Shanghai B&P Industries Co., Ltd.; Summary: the present invention relates to a kind of method utilizing Herba Eichhorniae to prepare bio-natural gas and biological dry ice, comprise the following steps: step one, by Herba Eichhorniae pre-treatment, pumped into marsh-gas fermentation tank afterwards to prepare biogas, remove hydrogen sulfide, carbon monoxide, nitrogen and the oxygen in biogas, for subsequent use; Step 2, prepares bio-natural gas and biological dry ice; By the gas filtration of step one gained, be compressed to 3.0 ~ 4.0MPaG afterwards, then by amine liquid carbon dioxide removal, molecular sieve dehydration, finally by mixed refrigeration process liquefaction, filling, obtain bio-natural gas; Collect aforementioned amine liquid, desorb, obtain carbonic acid gas, enter compressor, pressurized refrigerant through surge tank, cooling, obtains liquid carbon dioxide, i.e. biological dry ice.Method of the present invention is processed further and is prepared into bio-natural gas and dry ice on the basis of obtained biogas, has also increased substantially productivity effect while improve obtained biogas utilization rate.
Chinese patent, title:
"the method of gypsum prepared by a kind of Wingdale and Waste Sulfuric Acid and dry ice
"; Application Number (patent): CN200910038487.1; Applicant: Wang Jiaxing; Summary: the method that the invention discloses gypsum prepared by a kind of Wingdale and Waste Sulfuric Acid and dry ice.Its technical characteristics is: Wingdale and hydrochloric acid reaction generate calcium chloride and carbonic acid gas, carbonic acid gas dry ice and calcium chloride and Waste Sulfuric Acid continue to react the mixed solution generating white gypsum and hydrochloric acid, obtain filtrate hydrochloric acid after suction filtration to return last process and recycle and filter cake washing triple dewatering, dry, pulverize existing final gypsum product.The present invention not only effectively can reach the object of comprehensive regulation waste material, and, regional waste material can also reasonably avoid because simultaneously and deposit that there is lack of raw materials and cause the bad phenomenon that waste material can not be administered in time, and can not can create good economic worth for enterprise.
Chinese patent, title:
"lNG cold energy is utilized to prepare method and the device of Liquid carbon dioxide and dry ice
"; Application Number (patent): CN201410425132.9; Applicant: South China Science & Engineering University; Summary: the invention discloses the technique and the device thereof that utilize LNG cold energy to prepare Liquid carbon dioxide and dry ice.In described method: LNG pump enters the tube side of tube and shell heat exchanger, the gasification release latent heat of LNG in the tube side of tube and shell heat exchanger, by cryogenic gas CO
2cooling liquid, then the gasification product of LNG enters Multi-stream plate-fin heat exchanger as low-temperature receiver, CO
2cO is entered after unstripped gas cooling
2compressor, the high pressure-temperature CO simultaneously will exported
2cooling, LNG intensification gasification is the normal-temperature natural-gas of 10 ~ 25 DEG C; Cooled CO
2enter the shell of tube and shell heat exchanger, from the liquid CO that the outlet of tube and shell heat exchanger shell is flowed out
2be divided into two, one enters liquid CO
2storage tank, another enters dry-ice machine and prepares dry ice.This technique can realize the cascade utilization of LNG cold energy, and LNG cold energy use rate is high; By utilizing the cold energy of LNG by liquid CO
2and dry ice prepare Pressure Drop to 0.6 ~ 1.0MPa, and by compressor inlet gas CO
2be cooled to-40 ~-30 DEG C, finally can realize the effect of energy-conservation compared with pressure common method more than 58%.
Chinese patent, title:
"a kind of preparation method producing calcium metal
";application Number (patent): CN200910187892.X; Applicant: Xie Yansheng; Summary: a kind of preparation method producing calcium metal.The present invention is a kind of preparation method of calcium metal.It is by calcium oxide and aluminium powder and mineralizer, and by its proportioning, compacting balling-up, drops in vacuum electric donkey after drying and smelts, make its calcium oxide be reduced into calcium gas.Again calcium gas vacuum pump is extracted out, after cooling, manufacture calcium metal.It has less investment, cost is low, energy-conservation, reduce discharging advantage.
Applying hydrochloric acid in three strong acid when adopting chemical reaction method to produce carbonic acid gas and calcium metal, having extremely corrodibility, and discharge chlorine, chlorine band toxicity producing in calcium metal process, if can easily make people poisoning because of leaking, hindering HUMAN HEALTH, having the steady trouble of safety.
A lot of cities and counties, Guangxi belong to the mountain areas of karst landform, be rich in the distribution of the calcite in calcium carbonate ore deposit, Wingdale and rhombspar very general, rough estimates divide in each county, more than 77,835 hundred million tons are reached in this total resources that ground is exposed, especially be in and the calcite in Yunnan, mountain, boundary, Guizhou, detecting its chemical content up to 98.89% through metallurgical department, can exploit more than more than hundred year completely, is one of larger Mineral resources in Guangxi.
Calcite is a kind in calcium carbonate ore deposit, is also modal in natural whiting ore deposit.Its main component is by Ca(calcium), C(carbon), O(oxygen), three kinds of elements form, chemical equation is: CaCO
3, molecular weight 100.09, composition and content: CaO, 56.03%, CO
2, 43.9%, hardness: 3.0, proportion: 2.6 ~ 2.8, not containing other impurity elements, when its heat in: can split the carbon dioxide off when 819 ~ 832 degrees Celsius gas and calcium oxide.Therefore extracting carbon dioxide and calcium oxide for reaching, finally preparing solidified carbon dioxide, active metal calcium with physical method, having advantage richly endowed by nature.
Summary of the invention
There is continuity limitation in the commercial process of traditional chemical reaction method, for the ease of commercial process continuity, be beneficial to the enforcement of Automated condtrol operation, overcome existing production technology weak point, the invention provides a kind of calcite and prepare solidified carbon dioxide and calcium metal method, Bian is heated by resistive the calcining furnace that pipe is formed with far-infrared heating plate, take calcite as raw material, the product in early stage of carbon dioxide and calcium oxide is extracted with roasting physical method, then deep processing obtains solidified carbon dioxide, active metal calcium, production time-histories is shortened to reach, boost productivity, improve the quality of products, reduce production cost, finally reach increase economic interests, improve social benefit object.
Technical scheme of the present invention is:
Calcite prepares solidified carbon dioxide and calcium metal method, comprises the following steps:
(1) calcite is finally made the calcite stone flour of 1 ~ 3 millimeter through thick broken, thin broken;
(2) calcite stone flour is put into calcining furnace calcining and obtains calcium oxide and carbon dioxide;
(3) mixed with ferrosilicon powder by calcium oxide, carry out vacuum-thermal reduction reaction, gasification after reduction, displacement, distillation, disengages calcium steam, collects calcium steam and cools and obtain calcium metal solid and Calucium Silicate powder finished product;
Above-mentioned (1) step be by calcite after extraction, impurity elimination is cleaned with water, little building stones are slightly broken into jaw crusher, little building stones give by e Foerderanlage the fines that the further fragmentation of impact breaker obtains 2 ~ 3 centimetres, and fines gives by e Foerderanlage the stone flour that sand machine processed wears into 1 ~ 3 millimeter again.
Above-mentioned (2) step calcite stone flour calcining temperature is 800 ~ 900 DEG C.
The carbon dioxide that above-mentioned (2) step obtains is condensed into liquid carbon dioxide, the step making solidified carbon dioxide is further: calcite stone flour calcining cracking distils out the product in early stage of carbon dioxide and active calcium oxide, through dead front type pipeline, the carbonic acid gas of distillation is extracted out from stove upper plenum by vacuum pump again, do not send into the full automatic solid carbonic acid gas synthesis device of supporting installation with leaking, in this equipment under 5498 ~ 6250KPa pressure, carbon dioxide is condensed into colourless liquid carbon dioxide, under low pressure undergoes rapid expansion again, evaporate and generate solidified carbon dioxide finished product.
It is filling that the carbon dioxide that above-mentioned (2) step obtains also can be passed through pressurization condensation, obtains Liquid carbon dioxide.
(3) step calcium oxide powder and ferrosilicon powder by weight proportion 3:1 mix, and import in vacuum distillation furnace, calcium oxide mixes the condition of carrying out vacuum-thermal reduction reaction with ferrosilicon powder be temperature 1400-1600 DEG C, and pressure is 10Pa.
It is filling that the calcium steam that (3) step is collected also can be passed through pressurization condensation, obtains liquid calcium.
Calcite of the present invention is prepared solidified carbon dioxide and calcium metal method and is also applied to the material ore that the massfraction being added the total amount of calcium containing carbonate reaches more than 56%, comprises Wingdale, rhombspar, marble and chalk.
Compared with prior art, positively effect of the present invention is:
1, the present invention take calcite as raw material, carbon dioxide and active calcium oxide product in early stage is gone out through special sealing calcining furnace roasting cracking, then deep processing obtains solidified carbon dioxide and active metal calcium, solve the problem that local method lime kilning pollutes by the furnace gas such as coal, fuel, and calcite decomposes in special sealing calcining furnace and has that decomposition rate is fast, calcining temperature is low, the time is short, energy consumption is low, heat waste is little, lime whiteness is high, activity degree is high, hyperergic advantage.
2, the method for solidified carbon dioxide and calcium metal is prepared in calcite distillation of the present invention, the carbon dioxide that calcite obtains after calcining furnace cracking is extracted out through dead front type pipeline from stove upper plenum by vacuum pump, do not send into the full automatic solid carbonic acid gas synthesis device of supporting installation with leaking, be finally processed into solidified carbon dioxide.This technical process energy efficient recovery carbon dioxide, manufactures dry ice product, turns waste into wealth.
3, the present invention take calcite as raw material, is processed into calcium metal further with the lime that calcite obtains after calcining furnace cracking, increases product and adds the output value.Active calcium oxide extraction rate reached is to more than 60%.
4, in the process of the present invention does not produce chlorine, no "three wastes" emissions, no damage to human body, to the environment pollution-free, safe and reliable operation.
5, final product calcium metal of the present invention and water react and generate calcium hydroxide, discharge hydrogen, and calcium hydroxide can be reused through Footwall drift calcium.Hydrogen and dry ice, under catalyst action, can generate the nytron fuel of different components, and therefore resultant metal calcium and dry ice are the preposition products of hydrocarbon synthetic fuel, and market application foreground is wide, large to the potentiality tool substituting natural fossil fuel.
Accompanying drawing explanation
Fig. 1 calcite prepares the process flow sheet of solidified carbon dioxide and calcium metal.
Embodiment
Below in conjunction with embodiment, the present invention will be further described, but protection scope of the present invention is not limited to the scope that embodiment represents.
Embodiment 1
Calcite prepares solidified carbon dioxide and calcium metal method, comprises the following steps:
(1) calcite is finally made the calcite stone flour of 1 millimeter through thick broken, thin broken;
(2) calcite stone flour is put into calcining furnace calcining and obtains calcium oxide and carbon dioxide;
(3) mixed with ferrosilicon powder by calcium oxide, carry out vacuum-thermal reduction reaction, gasification after reduction, displacement, distillation, disengages calcium steam, collects calcium steam and cools and obtain calcium metal solid and Calucium Silicate powder finished product.
Above-mentioned (1) step be by calcite after extraction, impurity elimination is cleaned with water, slightly be broken into little building stones with jaw crusher, little building stones give by e Foerderanlage the fines that the further fragmentation of impact breaker obtains 2 centimetres, and fines gives by e Foerderanlage the stone flour that sand machine processed wears into 1 millimeter again.
Above-mentioned (2) step calcite stone flour calcining temperature is 800 DEG C.
The carbon dioxide that above-mentioned (2) step obtains is condensed into liquid carbon dioxide, the step making solidified carbon dioxide is further: calcite stone flour calcining cracking distils out the product in early stage of carbon dioxide and active calcium oxide, through dead front type pipeline, the carbonic acid gas of distillation is extracted out from stove upper plenum by vacuum pump again, do not send into the full automatic solid carbonic acid gas synthesis device of supporting installation with leaking, in this equipment under 5498KPa pressure, carbon dioxide is condensed into colourless liquid carbon dioxide, under low pressure undergoes rapid expansion again, evaporate and generate solidified carbon dioxide finished product.
It is filling that the carbon dioxide that above-mentioned (2) step obtains also can be passed through pressurization condensation, obtains Liquid carbon dioxide.
(3) step calcium oxide powder and ferrosilicon powder by weight proportion 3:1 mix, and import in vacuum distillation furnace, calcium oxide mixes the condition of carrying out vacuum-thermal reduction reaction with ferrosilicon powder be temperature 1400 DEG C, and pressure is 10Pa.
It is filling that the calcium steam that (3) step is collected also can be passed through pressurization condensation, obtains liquid calcium.
Embodiment 2
Calcite prepares solidified carbon dioxide and calcium metal method, comprises the following steps:
(1) calcite is finally made the calcite stone flour of 3 millimeters through thick broken, thin broken;
(2) calcite stone flour is put into calcining furnace calcining and obtains calcium oxide and carbon dioxide;
(3) mixed with ferrosilicon powder by calcium oxide, carry out vacuum-thermal reduction reaction, gasification after reduction, displacement, distillation, disengages calcium steam, collects calcium steam and cools and obtain calcium metal solid and Calucium Silicate powder finished product.
Above-mentioned (1) step be by calcite after extraction, impurity elimination is cleaned with water, slightly be broken into little building stones with jaw crusher, little building stones give by e Foerderanlage the fines that the further fragmentation of impact breaker obtains 3 centimetres, and fines gives by e Foerderanlage the stone flour that sand machine processed wears into 3 millimeters again.
Above-mentioned (2) step calcite stone flour calcining temperature is 900 DEG C.
The carbon dioxide that above-mentioned (2) step obtains is condensed into liquid carbon dioxide, the step making solidified carbon dioxide is further: calcite stone flour calcining cracking distils out the product in early stage of carbon dioxide and active calcium oxide, through dead front type pipeline, the carbonic acid gas of distillation is extracted out from stove upper plenum by vacuum pump again, do not send into the full automatic solid carbonic acid gas synthesis device of supporting installation with leaking, in this equipment under 6250KPa pressure, carbon dioxide is condensed into colourless liquid carbon dioxide, under low pressure undergoes rapid expansion again, evaporate and generate solidified carbon dioxide finished product.
It is filling that the carbon dioxide that above-mentioned (2) step obtains also can be passed through pressurization condensation, obtains Liquid carbon dioxide.
(3) step calcium oxide powder and ferrosilicon powder by weight proportion 3:1 mix, and import in vacuum distillation furnace, calcium oxide mixes the condition of carrying out vacuum-thermal reduction reaction with ferrosilicon powder be temperature 1600 DEG C, and pressure is 10Pa.
It is filling that the calcium steam that (3) step is collected also can be passed through pressurization condensation, obtains liquid calcium.
Claims (6)
1. calcite prepares solidified carbon dioxide and calcium metal method, it is characterized in that: comprise the following steps:
(1) calcite is finally made the calcite stone flour of 1 ~ 3 millimeter through thick broken, thin broken;
(2) calcite stone flour is put into calcining furnace calcining and obtains calcium oxide and carbon dioxide;
(3) mixed with ferrosilicon powder by calcium oxide, carry out vacuum-thermal reduction reaction, gasification after reduction, displacement, distillation, disengages calcium gas, collects calcium steam and cools and obtain calcium metal solid and Calucium Silicate powder finished product;
The carbon dioxide that above-mentioned (2) step obtains is condensed into liquid carbon dioxide, makes solidified carbon dioxide further.
2. calcite according to claim 1 prepares solidified carbon dioxide and calcium metal method, it is characterized in that: (1) step be by calcite after extraction, impurity elimination is cleaned with water, little building stones are slightly broken into jaw crusher, little building stones give by e Foerderanlage the fines that the further fragmentation of impact breaker obtains 2 ~ 3 centimetres, and fines gives by e Foerderanlage the stone flour that sand machine processed wears into 1 ~ 3 millimeter again.
3. calcite according to claim 1 prepares solidified carbon dioxide and calcium metal method, it is characterized in that: calcite stone flour calcining temperature is 800 ~ 900 DEG C.
4. calcite according to claim 1 prepares solidified carbon dioxide and calcium metal method, it is characterized in that: (3) step calcium oxide powder and ferrosilicon powder by weight proportion 3:1 mix, in importing vacuum distillation furnace, calcium oxide mixes the condition of carrying out vacuum-thermal reduction reaction with ferrosilicon powder be temperature 1400-1600 DEG C, and pressure is 10Pa.
5. calcite according to claim 1 prepares solidified carbon dioxide and calcium metal method, it is characterized in that: carbon dioxide is condensed into liquid carbon dioxide, the step making solidified carbon dioxide is further: calcite stone flour calcining cracking distils out the product in early stage of carbon dioxide and active calcium oxide, through dead front type pipeline, the carbonic acid gas of distillation is extracted out from stove upper plenum by vacuum pump again, do not send into the full automatic solid carbonic acid gas synthesis device of supporting installation with leaking, in this equipment under 5498 ~ 6250KPa pressure, carbon dioxide is condensed into liquid carbon dioxide, under low pressure undergoes rapid expansion again, evaporate and generate solidified carbon dioxide finished product.
6. calcite according to claim 1 prepares solidified carbon dioxide and calcium metal method, it is characterized in that: the method is also applied to the material ore that the massfraction of total amount being added calcium containing carbonate reaches more than 56%, comprises Wingdale, rhombspar, marble and chalk.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108342585A (en) * | 2018-03-13 | 2018-07-31 | 东北大学 | A kind of method of comprehensive utilization of magnesium-smelting reduction slag |
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