CN102602973B - Method for synthesizing ultrafine calcium carbonate by utilizing carbide slag - Google Patents
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- CN102602973B CN102602973B CN201210010874.6A CN201210010874A CN102602973B CN 102602973 B CN102602973 B CN 102602973B CN 201210010874 A CN201210010874 A CN 201210010874A CN 102602973 B CN102602973 B CN 102602973B
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Abstract
The invention relates to a method for synthesizing ultrafine calcium carbonate by utilizing carbide slag. The method comprises the following steps of: (1) dissolving carbide slag: uniformly mixing carbide slag with water in a ratio of (1:6)-(1:20) to ensure that the carbide slag is fully dissolved into a turbid liquid, wherein the water content of the carbide slag is 20-45%; (2) carrying out impregnation reaction: adding ammonium chloride into the turbid liquid of the carbide slag for uniformly mixing, wherein the mass ratio of carbide slag to ammonium chloride is (1:0.7)-(1:2.5), after the impregnation reaction is finished, filtering and removing the slag to obtain a clear calcium chloride solution; and (3) carrying out carbonization reaction: adding a crystal form control agent into a calcium chloride solution for fully dissolving, introducing CO2 into the solution to carry out carbonization reaction till the pH (potential of Hydrogen) value of the reaction solution is less than or equal to 7 to obtain ultrafine calcium carbonate slurry, wherein the crystal form control agent is one or more than two mixtures of sulfate, chloride, citrate, sodium dodecyl benzene sulfonate, pyrophosphate, oleic acid, ammonium citrate, N-methyl pyrrolidone and maleic acid.
Description
Technical field
The present invention relates to a kind of method of utilizing carbide slag synthesizing superfine calcium carbonate.
Background technology
Carbide slag is that chlorine industry utilizes calcium carbide to produce by product when acetylene gas, is a kind of trade waste.Statistics according to investigations, China produces every year carbide slag and approaches 4,000 ten thousand tons, and its utilization ratio less than 30%, for the production of cement, generally, all with land-fill method processing, not only take tract except on a small quantity, and alkalization soil, air and water source are caused to secondary pollution.
Along with the rapid growth of global economy, the sharply rising of energy consumption, " greenhouse gases " CO
2discharge rate along with people utilize can source speed increase and promptly increase, cause global warming.The calcining and decomposing of the burning of Cement industry mineral fuel and material carbon hydrochlorate all produces a large amount of CO
2if, only to consider with China's cement industry, the carbonic acid gas of annual discharge reaches several hundred million tons, and these carbonic acid gas run off in a large number in atmosphere, have not only brought great harm to environment, have also caused the significant wastage of carbon resource.
Calcium carbonate is a kind of important mineral filler, has been widely used in the industries such as rubber, plastics, coating, papermaking, ink, its applied range, and usage quantity is large, and added value is high.Therefore, utilize the technology of the light calcium carbonate of carbide slag and cement kiln end waste gas or power plant flue gas production high added value to be significant undoubtedly if develop.
The dry carbide slag water content of discharging in industry calcium carbide acetylene is 5～10%, and wet carbide slag water content is 30～40%.Patent CN1854069A through chloride leach solution, adds dried carbide slag sodium stearate after removing residue, then passes into CO
2gas, can obtain calcium carbonate tabular, spherical and three kinds of different crystal forms of needle-like by controlling temperature of reaction.Before this patent carbide slag reaction, need to be dried, energy consumption is high, and while preparing calcite type calcium carbonate, temperature of reaction need be controlled at 2～6 ℃, and this temperature of reaction needs refrigeration equipment.
Patent CN1058005A utilizes preparing high-purity technical calcium carbonate from calcium carbide dregs, this patent need be carried out pre-treatment to carbide slag, through carbide slag pre-heating drying at 150 ℃～200 ℃ of dehydration, 1201 ℃～1350 ℃ temperature lower calcinations 30～60 minutes, energy expenditure was larger.Although this patent has been produced highly purified calcium carbonate, to determining crystalline form and the size-grade distribution not mentioned of the most important parameter calcium carbonate particles that better function is bad.
Patent CN1085188A has proposed to manufacture with carbide slag the method for nm-class active calcium carbonate coproduction carbon dust, carbide slag is first carried out to pre-treatment, then carry out by a certain percentage purifying treatment with ammonium chloride again, after filtration, in clear liquor, add tensio-active agent and chemical additives, pass into CO
2gas carries out carbonization, finally obtains nm-class active calcium carbonate and carbon dust.This patent is used pure CO
2gas is source of the gas, has only provided the size of nm-class active calcium carbonate, as also not mentioned in whiteness, oil-absorption(number) and calcium oxide content to other important performance characteristic.
Patent CN1085188A has proposed with calcium carbide waste slag with containing lower concentration CO
2waste gas be that raw material generates the method for calcium carbonate, but the calcium carbide waste slag of the method needs calcining, digestion, refinement treatment.CO in the purifying treatment such as desulfurization and dedusting rear pass gas or kiln gas
2the content of gas is low, and volume ratio content is 5%～15%; And need under pressurized conditions, carry out carburizing reagent.Although this patent utilizes waste residue and waste gas to prepare calcium carbonate, complex process, need more equipment, and the content of carbonic acid gas is low, and the productive rate of calcium carbonate is low.Although this patent preparation lightweight and nano-calcium carbonate, but nano-calcium carbonate is because particle diameter is little, surface can be high, because very easily reuniting, the feature of surface hydrophilic oleophobic and strong polarity is disperseed inhomogeneously in organic medium, easily causes the boundary defect between base-material and filler, therefore need it to carry out surface activation process, improve nano-calcium carbonate surface property, regulate wettability and bonding force between hydrophobicity, raising and base-material.
Summary of the invention
The invention provides a kind of method of utilizing carbide slag synthesizing superfine calcium carbonate, this technique is simple, and carbide slag is without dry or calcining pretreatment.
The described method of utilizing carbide slag synthesizing superfine calcium carbonate comprises the steps:
1) carbide slag dissolves: the ratio that is 1: 6～1: 20 in mass ratio by carbide slag and water mixes, make carbide slag fully be dissolved into suspension liquid, described carbide slag is the carbide slag discharging in industrial calcium carbide acetylene, and water content is wherein 20%～45% (quality);
2) impregnation: ammonium chloride is joined in the suspension liquid of carbide slag and mix, the mass ratio of carbide slag and ammonium chloride is 1: 0.7～1: 2.5; After impregnation finishes, after filter cleaner, obtain the calcium chloride solution of clarification;
3) carburizing reagent: add crystal control agent in calcium chloride solution, fully dissolve in backward this solution and pass into CO
2carry out carburizing reagent, until the pH value of reaction soln is less than or equal to 7, obtain calcium carbonate superfine powder slurries, described crystal control agent is one or more mixtures in vitriol, muriate, Citrate trianion, Sodium dodecylbenzene sulfonate, pyrophosphate salt, oleic acid, ammonium citrate, N-Methyl pyrrolidone, maleic acid, and add-on is 0.1%～5.0% of the calcium carbonate quality that obtains of carburizing reagent.
Preferred steps 1) in be 1: 8～1: 10 in mass ratio by carbide slag and water ratio mixes, the water content of carbide slag is preferably 35%.
Preferred steps 2) in the mass ratio of carbide slag and ammonium chloride be 1: 0.7～1: 0.8.
Preferably crystal control agent is the mixture that N-Methyl pyrrolidone and the Sodium dodecylbenzene sulfonate mass ratio mixture that is 1: 1 or potassium pyrophosphate and Sodium dodecylbenzene sulfonate mass ratio are 2: 1, and the consumption of crystal control agent is preferably carburizing reagent and generates 1% of weight of calcium carbonate.
As improvement of the present invention, also comprise step 4) activation treatment: add activator to carry out liquid phase surface activation process in the calcium carbonate superfine powder slurries after carburizing reagent, super-fine active calcium carbide slurry is through dehydration, washing, dry, can obtain activated Calcium carbonate micro mist, described activator is one or more mixtures in lipid acid or water-soluble coupling agent, the activation dosage adding is 0.1%～5% of carburizing reagent gained calcium carbonate quality, described lipid acid is palmitinic acid, lauric acid, stearic acid, oleic acid, and the mixture of one or more arbitrary proportions in their salt, described water-soluble coupling agent is titanate, hydramine titan-alkoxide acid esters, hydramine lipid acid titanic acid ester, Aluminate, the mixture of one or more arbitrary proportions in silane coupling agent, preferred active agent is soluble silane coupling agent CG-151, or stearic acid sodium.Preferably, when liquid phase surface activation process, temperature is 50～95 ℃, and the treatment time is 0.5～3.5 hour, and more preferably liquid phase surface activation process temperature is 50～80 ℃, and the treatment time is 2～3.5 hours.The aqueous solution that activator can first melt into concentration is 5～20%, then add priming reaction system.When activator adds fashionablely with solution form, the consumption of above-mentioned activator refers to the quality of contained activator in solution.
Preferably, step 3) in pass into containing CO
2cement mill kiln tail gas or power plant flue gas carry out carburizing reagent, CO in described cement mill kiln tail gas or power plant flue gas
2content be 20%～45% (volume fraction), more preferably CO
2content be 30% (volume fraction).In order to obtain described CO
2cement mill kiln tail gas or the power plant flue gas of content, described cement mill kiln tail gas or power plant flue gas should carry out dedusting, absorption, cooling and solution-air isolation of purified process in advance.
Preferably, carbonation reaction temperature is 10～25 ℃, and pressure is normal pressure.
The waste water of the ammonia producing in steeping process or ammoniacal liquor and chloride ion-containing can be recycled after recycling, to meet the utilization of resources and environment protection control requirements, and/or by the waste residue giving off in steeping process of the present invention (iron content, aluminium, silicon etc.), utilize for manufacture of cement starting material after treatment, guarantee absolutely utilization ratio of waste residue.
The present invention has the following advantages: carbide slag transformation efficiency is high, and products obtained therefrom size distribution is even, and different batches product stability is good.Directly lipid acid and water-soluble coupling agent are joined in calcium carbonate suspension liquid, by stirring, lipid acid is fully contacted with nano-calcium carbonate with water-soluble coupling agent, activation evenly, improves its dispersiveness, increases affinity and the consistency of nano-calcium carbonate and organic medium.Micro powder product can reach the standard-required of industrial super-fine active calcium carbide (HG/T2776-1996), can be used as the functional stuffing in high-grade rubber, plastics and ink.CO in the waste gas of reduction of discharging cement mill
2when gas, also solve the problem of waste residue-carbide slag outlet difficulty in chemical industry for making chlorine and alkali.The present invention not only reduces and has administered the environmental pollution that waste residue and waste gas cause, and makes its resource utilization, and the Chemicals of synthetic high added value, have outstanding society and economic benefit.This technology had both met utilization of waste as resource policy, met again circular economy policy, was the particular embodiment of the raising resource utilization advocated at present and the innovation of low-carbon economy art.
Accompanying drawing explanation
Fig. 1 is the process flow sheet that embodiment 1-4 utilizes carbide slag and cement mill kiln tail gas or power plant flue gas synthesizing superfine activated Calcium carbonate micro mist.
Embodiment
Embodiments of the invention are as follows:
Embodiment 1
The carbide slag that is 35% by water content and water are that the ratio of 1: 10 mixes in mass ratio, make carbide slag fully be dissolved into suspension liquid, in the suspension of carbide slag, add ammonium chloride fully to react, the pH value of controlling solution is more than or equal to 7, the mass ratio of carbide slag and ammonium chloride is 1: 0.78, after removing residue, add crystal control agent N-Methyl pyrrolidone and Sodium dodecylbenzene sulfonate (mass ratio is 1: 1), the add-on of controlling crystal control agent is 1% of carburizing reagent generation weight of calcium carbonate, and then contains CO after passing into purification
2gas (CO
2volume percent be 30%) cement mill kiln tail gas or power plant flue gas carry out carbonization, and the temperature of controlling carburizing reagent is 10～25 ℃, until the pH value of solution is less than or equal to 7, calcium carbonate superfine powder slurries after carburizing reagent are carried out to liquid phase surface activation process, activation temperature is 80 ℃, soak time 2 hours, activator is sodium stearate, add-on is 2% of carburizing reagent generation weight of calcium carbonate, through dehydration, washing, be dried and can obtain light calcium carbonate fine powder, carbide slag transformation efficiency is 72%, calcium carbonate product detected result shows, crystalline form is spherical calcium carbonate, single particle median size is 60～80nm, gained calcium oxide content is 53.2%, specific surface area 35m
2/ g, oil-absorption(number) 30DOP/100CaCO
3, other performance meets industrial super-fine active calcium carbide (HG/T2776-1996) standard-required.
Embodiment 2
The carbide slag that is 35% by water content and water are that the ratio of 1: 10 mixes in mass ratio, make carbide slag fully be dissolved into suspension liquid, in the suspension of carbide slag, add ammonium chloride fully to react, the pH value of controlling solution is more than or equal to 7, the mass ratio of carbide slag and ammonium chloride is 1: 0.78, after removing residue, add crystal control agent N-Methyl pyrrolidone and Sodium dodecylbenzene sulfonate (mass ratio is 1: 1), the add-on of controlling crystal control agent is 1% of carburizing reagent generation weight of calcium carbonate, and then contains CO after passing into purification
2gas (CO
2volume percent be 30%) cement mill kiln tail gas or power plant flue gas carry out carbonization, and the temperature of controlling reaction is 10～25 ℃, until the pH value of solution is less than or equal to 7, calcium carbonate superfine powder slurries after carburizing reagent are carried out to liquid phase surface activation process, activation temperature is 50 ℃, soak time 2 hours, activator is sodium stearate, add-on is 1% of carburizing reagent generation weight of calcium carbonate, through dehydration, washing, be dried and can obtain light calcium carbonate fine powder, carbide slag transformation efficiency is 72%, calcium carbonate product detected result shows, crystalline form is chain calcium carbonate, single particle median size is 70～90nm, gained calcium oxide content is 52%, specific surface area 28m
2/ g, oil-absorption(number) 32DOP/100CaCO
3, other performance meets industrial super-fine active calcium carbide (HG/T2776-1996) standard-required.
Embodiment 3
The carbide slag that is 35% by water content and water are that the ratio of 1: 9 mixes in mass ratio, make carbide slag fully be dissolved into suspension liquid, in the suspension of carbide slag, add ammonium chloride fully to react, the pH value of controlling solution is more than or equal to 7, the mass ratio of carbide slag and ammonium chloride is 1: 0.78, after removing residue, add crystal control agent potassium pyrophosphate and Sodium dodecylbenzene sulfonate (mass ratio is 2: 1), the add-on of controlling crystal control agent is 1% of carburizing reagent generation weight of calcium carbonate, and then contains CO after passing into purification
2gas (CO
2volume percent be 30%) cement mill kiln tail gas or power plant flue gas carry out carbonization, and the temperature of controlling reaction is 10～25 ℃, until the pH value of solution is less than or equal to 7, calcium carbonate superfine powder slurries after carburizing reagent are carried out to liquid phase surface activation process, activation temperature is 70 ℃, soak time 2 hours, activator is soluble silane coupling agent CG-151 (Jiangsu Chenguang Coincident Dose Co., Ltd.), activator add-on is 1% of carburizing reagent generation weight of calcium carbonate, it is that 5% the aqueous solution adds again that activator is first mixed with concentration, through dehydration, washing, be dried and can obtain light calcium carbonate fine powder, carbide slag transformation efficiency is 75%, calcium carbonate product detected result shows, crystalline form is chain calcium carbonate, single particle median size is 50～80nm, gained calcium oxide content is 54.3%, specific surface area 25m
2/ g, oil-absorption(number) 25DOP/100CaCO
3, other performance meets industrial super-fine active calcium carbide (HG/T2776-1996) standard-required.
Embodiment 4
The carbide slag that is 35% by water content and water are that the ratio of 1: 9 mixes in mass ratio, make carbide slag fully be dissolved into suspension liquid, in the suspension of carbide slag, add ammonium chloride fully to react, the pH value of controlling solution is more than or equal to 7, the mass ratio of carbide slag and ammonium chloride is 1: 0.78, after removing residue, add crystal control agent potassium pyrophosphate and Sodium dodecylbenzene sulfonate (mass ratio is 2: 1), the add-on of controlling crystal control agent is 1% of carburizing reagent generation weight of calcium carbonate, and then contains CO after passing into purification
2gas (CO
2volume percent be 30%) cement mill kiln tail gas or power plant flue gas carry out carbonization, and the temperature of controlling reaction is 10～25 ℃, until the pH value of solution is less than or equal to 7, calcium carbonate superfine powder slurries after carburizing reagent are carried out to liquid phase surface activation process, activation temperature is 70 ℃, soak time 3.5 hours, activator is soluble silane coupling agent CG-151 (Jiangsu Chenguang Coincident Dose Co., Ltd.), activator add-on is 1% of carburizing reagent generation weight of calcium carbonate, it is that 20% the aqueous solution adds again that activator is first mixed with concentration, through dehydration, washing, be dried and can obtain light calcium carbonate fine powder, carbide slag transformation efficiency is 75%, calcium carbonate product detected result shows, crystalline form is chain calcium carbonate, single particle median size is 40～70nm, gained calcium oxide content is 53.6%, specific surface area 27m
2/ g, oil-absorption(number) 20DOP/100CaCO
3, other performance meets industrial super-fine active calcium carbide (HG/T2776-1996) standard-required.
Claims (4)
1. a method of utilizing carbide slag synthesizing superfine calcium carbonate, is characterized in that, comprises the steps:
1) carbide slag dissolves: in mass ratio for the ratio of 1:6～1:20 mixes, make carbide slag fully be dissolved into suspension liquid in carbide slag and water, described carbide slag is the carbide slag discharging in industrial calcium carbide acetylene, and water content is wherein 20wt%～45wt%;
2) impregnation: ammonium chloride is joined in the suspension liquid of carbide slag and mix, the mass ratio of carbide slag and ammonium chloride is 1:0.7～1:2.5; After impregnation finishes, after filter cleaner, obtain the calcium chloride solution of clarification;
3) carburizing reagent: add crystal control agent in calcium chloride solution, fully dissolve in backward this solution and pass into CO
2carry out carburizing reagent, until the pH value of reaction soln is less than or equal to 7, obtain calcium carbonate superfine powder slurries, described crystal control agent is one or more mixtures in vitriol, muriate, Citrate trianion, Sodium dodecylbenzene sulfonate, pyrophosphate salt, oleic acid, N-Methyl pyrrolidone, maleic acid, and add-on is 0.1%～5.0% of the calcium carbonate quality that obtains of carburizing reagent;
4) activation treatment: add activator to carry out liquid phase surface activation process in the calcium carbonate superfine powder slurries after carburizing reagent, gained super-fine active calcium carbide slurry is through dehydration, washing, dry, can obtain activated Calcium carbonate micro mist, described activator is one or more mixtures in lipid acid or its salt or water-soluble coupling agent, add-on is 0.1%～5% of carburizing reagent gained calcium carbonate quality, described lipid acid is palmitinic acid, lauric acid, stearic acid, the mixture of one or more arbitrary proportions in oleic acid, described water-soluble coupling agent is titanate, hydramine titan-alkoxide acid esters, hydramine lipid acid titanic acid ester, Aluminate, the mixture of one or more arbitrary proportions in silane coupling agent.
2. the method for utilizing carbide slag synthesizing superfine calcium carbonate as claimed in claim 1, is characterized in that, when liquid phase surface activation process, temperature is 50～95 ℃, and the treatment time is 0.5～3.5 hour, and activator is that concentration is 5～20% the aqueous solution.
3. the method for utilizing carbide slag synthesizing superfine calcium carbonate as claimed in claim 1 or 2, is characterized in that, passes into containing CO
2cement mill kiln tail gas or power plant flue gas carry out carburizing reagent, CO in described cement mill kiln tail gas or power plant flue gas
2volume fraction content be 20%～45%.
4. the method for utilizing carbide slag synthesizing superfine calcium carbonate as claimed in claim 3, is characterized in that, carbonation reaction temperature is 10～25 ℃, and pressure is normal pressure.
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