CN1218877C - Preparation method of cubic ultrafine precipitated calcium carbonate - Google Patents
Preparation method of cubic ultrafine precipitated calcium carbonate Download PDFInfo
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- CN1218877C CN1218877C CN 03116046 CN03116046A CN1218877C CN 1218877 C CN1218877 C CN 1218877C CN 03116046 CN03116046 CN 03116046 CN 03116046 A CN03116046 A CN 03116046A CN 1218877 C CN1218877 C CN 1218877C
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Abstract
The present invention provides a preparation method of cubic ultra-fine precipitated calcium carbonate, which is characterized in that lime milk after aging for 48 hours is added to a composite chelating agent after a soluble processing. The lime milk is led with an appropriate flow capacity of CO2 to carry out a carburizing reagent, the reaction temperature is controlled to be between 40 to 60 DEG C after rising, and the whole process of the reaction is traced by a conductivity apparatus. The lime milk is added with organic dispersing agent until reacting completely when the carbonized rate is 50 to 80%. The cubic crystalline precipitate calcium carbonate is obtained after filtration and drying of the product. The present invention has the characteristics of low cost, low energy consumption, narrow and thin distribution of the average sized particles, easy control of reaction process, etc.
Description
Technical field
The present invention relates to a kind of preparation method of cube ultra-fine precipitates lime carbonate of economy, affiliated technical field is preparation inorganic and that solid material is chemical.
Background technology
Lime carbonate is one of the widest Inorganic Chemicals of present purposes, because price is low, raw material is wide, and nontoxicity is widely used in industries such as rubber, plastics, coating, papermaking, daily-use chemical industry and does weighting agent and reinforcement, semi-reinforcing agent.Along with the progress of domestic miniaturization and process for treating surface, make calcium carbonate product to specialized, become more meticulous, the functionalization development, the Application Areas of lime carbonate has been expanded in arising at the historic moment of novel material calcium carbonate superfine powder product.
Produce with remaining of chemical process large-scale industrial production precipitated chalk in the world at present with carborization.Be about to the kiln gas (CO that calcined limestone produces
2) feeding the heterogeneous carburizing reagent of carrying out solid, liquid, gas in the certain density milk of lime slurry, this reaction is thermodynamic (al) exothermal reaction process.As allow carburizing reagent in opening wide reactor, carry out, to temperature if the words do not controlled, will cause the temperature of reaction system to continue to rise so, can rise until about 80 ℃ from room temperature, the precipitated chalk product crystalline form that obtains will be mainly spindle shape and amorphous etc., and wide in rangeization of particle diameter, end-use is restricted.Present suitability for industrialized production cube type ultra-fine precipitates calcium carbonate product, all under less than 25 ℃ of conditions, carry out, carburizing reagent need be cooled off temperature control and just can be carried out, the result is a subcooling process energy consumption height, prepared cube ultra-fine precipitates calcium carbonate product surface energy is also high, Intermolecular Forces is big, and then causes viscosity excessive.If be reflected at greater than carrying out carburizing reagent under 35 ℃ the constant temperature, do not carry out special chemistry, when physical technology is handled, then the crystalline form of product still be the fusiform product, be the product cut size scope become narrow controlled.Therefore, preparation cube type ultra-fine precipitates lime carbonate under high temperature (〉=40 ℃) condition is developed, the refrigerating apparatus of enterprise is reduced, power consumption reduces, thereby has saved the energy for the temperature control additive decrementation.
Chinese patent (publication number CN-1361063A) has been introduced the method that the one step carbonization of a kind of usefulness prepares cubic calcium carbonate, it is characterized in that with methyl polyoxy silane being that the compound crystal control agent of main body comes synthesis of cubic lime carbonate.
Chinese patent (publication number CN-1169955A) has been introduced a kind of method that is used to prepare the ultra-fine precipitates calcium carbonate granule, and this method divided for two steps carried out: the first step makes about 0.04 micron colloid lime carbonate with chemical method; The product of second step with the first step is crystal seed, crystal seed added carry out carburizing reagent in the milk of lime, and institute's synthetic lime carbonate is that particle diameter is 0.1～1 micron a cube product.
The precipitated chalk preparation method that above-mentioned patent is introduced all exists or control agent cost height, or the technology relative complex, and size distribution is the characteristics of narrow refinement inadequately.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of cube ultra-fine precipitates lime carbonate of economy.Method of the present invention has that cost, energy consumption are low, the narrow refinement of average particle size distribution and the more manageable characteristics of reaction process.
The invention provides the method for preparation cube ultra-fine precipitates lime carbonate, in 48 hours lime slurry of ageing, add the composite chelate agent of handling through processable, feed the CO of desired flow
2Carry out carburizing reagent, temperature of reaction rises the back Controllable Temperature built in 40～60 ℃, follows the tracks of the reaction whole process with conductivity meter.Carbonation rate added organic dispersing agent until reacting completely at 50～80% o'clock.Product after filtration, after the drying, obtain the cubic-crystal precipitated chalk.
Above-mentioned composite chelate agent is: disodium EDTA: sodium bicarbonate, weight ratio are 0.01～10: 1, or Diethylenetriamine penta acetate: sodium bicarbonate, weight ratio are 0.01～10: 1.
Above-mentioned composite chelate agent consumption is 0.01～10wt%, is benchmark with the theoretical growing amount of lime carbonate.
Above-mentioned lime slurry is the suspension liquid of calcium hydroxide, and its concentration is controlled at 10～30wt%.Reaction is at room temperature carried out.
Above-mentioned being reflected under 1000～2000 rev/mins the violent stirring slowly adds the composite chelate agent of handling through processable continuously, the composite chelate agent add finish after, further stir 3～40min.
Described organic dispersing agent is polyoxyethylene glycol or diethanolamine or sodium polyacrylate, and its add-on is 0.01～10wt% of the theoretical growing amount of lime carbonate.
The described carburizing reagent deadline is 20～300 minutes.
Above-mentioned reaction feeds 5～45% (v/v) CO
2Carry out carburizing reagent, after temperature of reaction rose, Controllable Temperature was carried out isothermal reaction built in certain point of 40～60 ℃.Carbonation rate added organic dispersing agent until reacting completely at 50～80% o'clock.Follow the tracks of the reaction whole process with conductivity meter.When final conductivity data rises slightly, show that this carburizing reagent finishes.Final product is through ageing, filtration, drying and other steps and obtain.
In the process of preparation provided by the present invention cube ultra-fine precipitates lime carbonate, the composite chelate agent has been carried out the solubility of water and handled.On the one hand the composite chelate agent can be rapidly mixes with milk of lime in the reaction system, reaches maximum point-to-point contact; Calcium ion huge legendary turtle in the reaction system is closed on the other hand, the lime carbonate crystal seed generates and heterogeneous reaction in the dynamic diffusion reaction, impel the crystalline process of growth controlled.
In the reaction system of preparation provided by the present invention cube ultra-fine precipitates lime carbonate, CO
2In carbonization process, obtained sufficient exchange, its CO
2Total flux is controlled at 1～100L/minKg Ca (OH)
2
The method of carburizing reagent preparation cube ultra-fine precipitates lime carbonate provided by the present invention, its advantage is: the composite chelate agent be easy to get and the energy consumption narrow refinement of average particle size distribution low, product cheap, reaction process and reaction process more easy to control, thereby adopt this method to carry out cube production of ultra-fine precipitates lime carbonate and can improve economic benefit of enterprises preferably.
Embodiment
Embodiment 1
At first, get and contain 10～30wt% milk of lime 500mL, under 1000～2000 rev/mins violent stirring, add the composite chelate agent disodium EDTA of handling through processable: sodium bicarbonate or Diethylenetriamine penta acetate: the intercalating agent of sodium bicarbonate, composite chelate agent consumption are to be 0.01～10wt% of datum quantity with the theoretical growing amount of lime carbonate.After composite chelate agent adding finishes, further stir 3～40min.Feed CO down at 20 ℃ then
2, CO
2Total flux is controlled at 1～5L/min Kg Ca (OH)
2After temperature of reaction rose, Controllable Temperature was carried out isothermal reaction built in certain point of 40～60 ℃.Carbonation rate added organic dispersing agent until reacting completely at 50～80% o'clock.Follow the tracks of the reaction whole process with conductivity meter.When final conductivity data rose slightly, carburizing reagent finished.Product is obtained through ageing, filtration, drying etc.Every index to product is measured, and its crystalline form is a cubes, and laser particle analyzer records the product cut size scope at 0.8～1.5 micron.Scanning electronic microscope shows that its size is 0.1 micron, and size distribution is even.
Embodiment 2
With with embodiment 1 identical operations, difference be with starting temperature 27 ℃ begin the reaction.
Finally every index of product is measured, shown that its crystalline form is a cubes, laser particle analyzer records the product cut size scope at 1.8～2.0 μ m.Scanning electronic microscope shows that its size is 0.3 micron, and size distribution is even.
Embodiment 3
With with embodiment 1 identical operations, difference is CO
2Total flux increases to 6～100L/minKg Ca (OH)
2, outlet temperature is controlled at 40 ℃.
Its crystalline form of the calcium carbonate product that is obtained is a cubes, and scanning electronic microscope shows that its size is 80nm, and laser particle analyzer records the product cut size scope at 1.2～2.0 microns.The narrow refinement of average particle size distribution.
Claims (4)
1, the preparation method of a kind of cube of ultra-fine precipitates lime carbonate, it is characterized in that in 48 hours milk of lime of ageing, adding the composite chelate agent of handling through processable, its composite chelate agent is: disodium EDTA: sodium bicarbonate, weight ratio is 0.01～10: 1, or Diethylenetriamine penta acetate: sodium bicarbonate, weight ratio is 0.01～10: 1, feeds the CO of desired flow
2Carry out carburizing reagent, temperature was controlled at 4 0～60 ℃ after temperature of reaction rose, follow the tracks of the reaction whole process with conductivity meter, carbonation rate added organic dispersing agent at 50～80% o'clock, and described organic dispersing agent is polyoxyethylene glycol or diethanolamine or sodium polyacrylate, add-on is 0.01～10wt% of the theoretical growing amount of lime carbonate, until reacting completely, product after filtration, after the drying, obtain the cubic-crystal precipitated chalk.
According to the preparation method of described cube of ultra-fine precipitates lime carbonate of claim 1, it is characterized in that 2, described lime milk concentration is 10～30wt%.
According to the preparation method of described cube of ultra-fine precipitates lime carbonate of claim 1, it is characterized in that 3, described composite chelate agent consumption is 0.01～10wt%, is benchmark with the theoretical growing amount of lime carbonate.
According to the preparation method of described cube of ultra-fine precipitates lime carbonate of claim 1, it is characterized in that 4, the described carburizing reagent deadline is 20～300 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03116046 CN1218877C (en) | 2003-03-26 | 2003-03-26 | Preparation method of cubic ultrafine precipitated calcium carbonate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03116046 CN1218877C (en) | 2003-03-26 | 2003-03-26 | Preparation method of cubic ultrafine precipitated calcium carbonate |
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| CN1513764A CN1513764A (en) | 2004-07-21 |
| CN1218877C true CN1218877C (en) | 2005-09-14 |
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| CN 03116046 Expired - Fee Related CN1218877C (en) | 2003-03-26 | 2003-03-26 | Preparation method of cubic ultrafine precipitated calcium carbonate |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7468101B2 (en) * | 2006-08-17 | 2008-12-23 | Specialty Minerals (Michigan) Inc. | UV varnish gloss performance using novel pigment and process for making same |
| CN103880058B (en) * | 2014-03-26 | 2016-01-20 | 河北工业大学 | A kind of precipitated chalk production technique of falling magnesium increasing calcium |
| CN103897434B (en) * | 2014-04-19 | 2016-03-30 | 芮城新泰纳米材料有限公司 | The preparation method that plastic master batch is Nano calcium carbonate dedicated |
| CN109437273B (en) * | 2018-12-19 | 2020-09-08 | 广西合山市华纳新材料科技有限公司 | Preparation method of monodisperse cubic precipitated calcium carbonate |
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