CN101983924B - Method for preparing calcium carbonate with controllable topography by using calcium sulfate - Google Patents
Method for preparing calcium carbonate with controllable topography by using calcium sulfate Download PDFInfo
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- CN101983924B CN101983924B CN2010105674426A CN201010567442A CN101983924B CN 101983924 B CN101983924 B CN 101983924B CN 2010105674426 A CN2010105674426 A CN 2010105674426A CN 201010567442 A CN201010567442 A CN 201010567442A CN 101983924 B CN101983924 B CN 101983924B
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Abstract
The invention provides a method for preparing calcium carbonate with controllable topography by taking calcium sulphate as calcium resource, and the topography of calcium carbonate comprises fusiformis, sphere, rod shape and the like. The invention is characterized in that calcium sulphate which is slightly soluble to water is dispersed in N, N-dimethyl formamide or absolute ethyl alcohol to form suspension solution; carbonate solution is added to react for certain time to decentralize and separate products; after the product is dispersed to deionized water to be stirred for certain time, the product is decentralized, washed and dried to obtain single-phase calcium carbonate powder. The topography of the product can be controlled by changing preparation conditions, such as reaction temperature, reaction time, reactant density and dissolved solvent and the like. The method has the characteristics of cheap raw material, simple technology, simple operation, controllable topography and the like.
Description
Technical field
The invention belongs to inorganic salt material technology field, relate to the preparation method of the controlled lime carbonate of a kind of pattern.
Background technology
Lime carbonate is as a kind of important inorganic non-metallic mineral material; In industry, be widely used as the filler of industries such as coating, papermaking, rubber, printing ink, plastics; The manufacturing raw material of organic synthesis, metallurgy, glass, pottery, medicine, food, makeup etc. also can be used for Industrial Wastewater Treatment, gastroduodenal ulcer sick acid inhibition, acidosic toxinicide, contains SO
2Removers etc. are a kind of very important inorganic chemical products.
The research of the controlled preparation lime carbonate of pattern is attracting the concern of many researchers, and the compound method that adopts at present mainly contains two kinds: the carborization and the precipitator method.Carborization is to adopt limestone calcination, lime slaking to obtain calcium hydroxide, in calcium hydroxide, feeds CO again
2Carry out technologies such as carbonization, separation, drying and produce lime carbonate.With Carbonization Preparation lime carbonate is the normal method that adopts of large-scale commercial prodn, but adopts this method to have the unmanageable problem of pattern, thus at present to the pattern of lime carbonate controlled preparation mainly adopt the precipitator method.The precipitator method are to adopt water-soluble Ca salt and water soluble carbonate under proper technical conditions, to react.Study more be in system, introduce tensio-active agent or superpolymer etc. or with the free calcium ions complexing, thereby perhaps in solution, form forming core and the process of growth that certain structure influence lime carbonate, the lime carbonate of acquisition different-shape.The present invention attempts to use the calcium sulfate that is slightly soluble in water as the calcium source, and with N, dinethylformamide or absolute ethyl alcohol are solvent dispersion calcium source, form suspension of calcium sulfate, avoids directly adopting in traditional precipitator method the calcium salt of solubility; Introduce carbonate on this basis,, calcium sulfate is slowly dissolved separate out calcium ion, combine to form calcium carbonate powder with carbanion, control the pattern of lime carbonate through the control reaction conditions along with the increase that adds the water yield in the carbonate aqueous solution.React incomplete situation for calcium sulfate, what this technological process obtained is the mixture of lime carbonate and calcium sulfate, this mixture is dissolved in to stir certain hour in the appropriate amount of deionized water be the sour calcium of sulfur dissolving, obtains single-phase lime carbonate.This technology need not add tensio-active agent and polymkeric substance, can simplify preparation technology, practices thrift cost, in suitability for industrialized production, has important realistic function.
Summary of the invention
The object of the present invention is to provide a kind of method for preparing the controlled lime carbonate of pattern with calcium sulfate for the calcium source.The calcium sulphate powders that is slightly soluble in water is dispersed in N; Form the calcium sulfate aaerosol solution in dinethylformamide or the absolute ethyl alcohol; Adding concentration is the carbonate solution 20-80 ℃ of reaction 1-12h of 0.01mol/L-0.9mol/L; Product is centrifugal and be distributed in the 50-1000mL deionized water, stir behind the 1-8h centrifuge washing and handle and obtain the controlled single-phase calcium carbonate powders of pattern.The method that is provided is simple, and is easy to operate, and used low in raw material cost is easy to get, and is a kind of preparation method who is suitable for suitability for industrialized production.Concrete steps are:
(1) the calcium sulphate powders magnetic agitation with prepared fresh is scattered in 50mL N, forms aaerosol solution in dinethylformamide or the absolute ethyl alcohol;
(2) add sodium hydrogencarbonate or the sodium carbonate solution that 50mL concentration is 0.01mol/L-0.9mol/L, 20-80 ℃ of stirring reaction 1-12h fast;
(3) will precipitate centrifugal and be transferred in the beaker, add the 50-1000mL deionized water, at room temperature magnetic agitation 1-8h;
(4) product in the liquid-phase system is separated, separated products is washed and drying treatment, promptly get calcium carbonate powder.
Compared with prior art, the invention has the advantages that:
(1) the present invention is the calcium source through selecting for use the calcium sulfate that is slightly soluble in water to replace nitrocalcite or calcium chloride soluble in water; At first it is scattered in N; Form aaerosol solution in dinethylformamide or the absolute ethyl alcohol, the increase through the water yield impels the slow dissolving of calcium sulfate to discharge calcium ion to participate in reaction and form lime carbonate.
(2) prepared lime carbonate crystalline phase purity is high, morphology control is more even.Change pattern with reaction conditions presents variety, comprises fusiformis, sphere and bar-shaped etc.
(3) reaction raw materials is simple and cheap and easy to get, need not add tensio-active agent or complexing agent, and the preparation method is simple, and reaction conditions is easy to control, does not need cost and complex equipment, is easy to realize suitability for industrialized production.
Description of drawings
X-ray powder diffraction (XRD) collection of illustrative plates of the lime carbonate of Fig. 1, embodiment 1 preparation.
ESEM (SEM) photo of the lime carbonate of Fig. 2, embodiment 1 preparation.
ESEM (SEM) photo of the lime carbonate of Fig. 3, embodiment 2 preparations.
ESEM (SEM) photo of the lime carbonate of Fig. 4, embodiment 3 preparations.
X-ray powder diffraction (XRD) collection of illustrative plates of the lime carbonate of Fig. 5, embodiment 4 preparations.
ESEM (SEM) photo of the lime carbonate of Fig. 6, embodiment 4 preparations.
ESEM (SEM) photo of the lime carbonate of Fig. 7, embodiment 5 preparations.
ESEM (SEM) photo of the lime carbonate of Fig. 8, embodiment 6 preparations.
Below in conjunction with accompanying drawing and embodiment the present invention is described further, but protection scope of the present invention is not limited only to following embodiment.
Embodiment
Embodiment 1
The calcium sulfate precursor magnetic agitation of prepared fresh is dispersed in 50mL N, and in the dinethylformamide, temperature is 35 ℃; With 50mL0.06mol/L NaHCO
3Solution is poured in the suspension-s fast, 35 ℃ of stirring reactions 4 hours; To precipitate centrifugal and be transferred in the beaker, and add 200ml zero(ppm) water, at room temperature magnetic agitation is 3 hours; Separated products is carried out centrifugal, washing and drying treatment, promptly get calcium carbonate powder.Fig. 1 is the X-ray powder diffraction result, shows that it is monophasic lime carbonate.Can find out that from the electron scanning micrograph of Fig. 2 it is fusiformis and flower-shaped mixing pattern.
Embodiment 2
The calcium sulfate precursor magnetic agitation of prepared fresh is dispersed in 50mL N, and in the dinethylformamide, temperature is 35 ℃; With 50mL0.18mol/L NaHCO
3Solution is poured in the suspension-s fast, 35 ℃ of stirring reactions 4 hours; To precipitate centrifugal and be transferred in the beaker, and add 200ml zero(ppm) water, at room temperature magnetic agitation is 3 hours; Separated products is carried out centrifugal, washing and drying treatment, promptly get calcium carbonate powder.Fig. 3 is its electron scanning micrograph, can find out clearly that it is mainly fusiformis lime carbonate.
Embodiment 3
The calcium sulfate precursor magnetic agitation of prepared fresh is dispersed in 50mL N, and in the dinethylformamide, temperature is 35 ℃; With 50mL0.06mol/L NaHCO
3Solution is poured in the suspension-s fast, 60 ℃ of stirring reactions 4 hours; To precipitate centrifugal and be transferred in the beaker, and add 200ml zero(ppm) water, at room temperature magnetic agitation is 3 hours; Separated products is carried out centrifugal, washing and drying treatment, promptly get calcium carbonate powder.Fig. 4 is its electron scanning micrograph, can find out clearly that it is mainly spherical calcium carbonate.
Embodiment 4
The calcium sulfate precursor magnetic agitation of prepared fresh is dispersed in 50mL N, and in the dinethylformamide, temperature is 35 ℃; With 50mL0.06mol/LNa
2CO
3Solution is poured in the suspension-s fast, 35 ℃ of stirring reactions 4 hours; To precipitate centrifugal and be transferred in the beaker, and add 200ml zero(ppm) water, at room temperature magnetic agitation is 3 hours; Separated products is carried out centrifugal, washing and drying treatment, promptly get calcium carbonate powder.Fig. 5 is the X-ray powder diffraction result, shows that it is monophasic lime carbonate.Can find out that from the electron scanning micrograph of Fig. 6 it is bar-shaped pattern.
Embodiment 5
The calcium sulfate precursor magnetic agitation of prepared fresh is dispersed in 50mLN, and in the dinethylformamide, temperature is 35 ℃; With 50mL0.12mol/LNa
2CO
3Solution is poured in the suspension-s fast, 35 ℃ of stirring reactions 4 hours; To precipitate centrifugal and be transferred in the beaker, and add 200ml zero(ppm) water, at room temperature magnetic agitation is 3 hours; Separated products is carried out centrifugal, washing and drying treatment, promptly get calcium carbonate powder.Fig. 7 is its electron scanning micrograph, can find out clearly that it is mainly the calcium carbonate granule that lamella piles up formation.
Embodiment 6
The calcium sulfate precursor magnetic agitation of prepared fresh is dispersed in the 50mL absolute ethyl alcohol, and temperature is 35 ℃; With 50mL0.12mol/L Na
2CO
3Solution is poured in the suspension-s fast, 60 ℃ of stirring reactions 4 hours; To precipitate centrifugal and be transferred in the beaker, and add 200ml zero(ppm) water, at room temperature magnetic agitation is 3 hours; Separated products is carried out centrifugal, washing and drying treatment, promptly get calcium carbonate powder.Fig. 8 is its electron scanning micrograph, can find out clearly that it is mainly the spherical calcium carbonate powder.
Claims (1)
1. a calcium sulfate transforms the method for preparing the controlled lime carbonate of pattern, it is characterized in that may further comprise the steps:
(1) the calcium sulphate powders magnetic agitation with prepared fresh is scattered in 50mL N, forms aaerosol solution in dinethylformamide or the absolute ethyl alcohol;
(2) add sodium hydrogencarbonate or the sodium carbonate solution that 50mL concentration is 0.01mol/L-0.9mol/L, 20-80 ℃ of stirring reaction 1-12h fast;
(3) will precipitate centrifugal and be transferred in the beaker, add the 50-1000mL deionized water, at room temperature magnetic agitation 1-8h;
(4) product in the liquid-phase system is separated, separated products is washed and drying treatment, promptly get calcium carbonate powder.
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| CN2010105674426A CN101983924B (en) | 2010-11-24 | 2010-11-24 | Method for preparing calcium carbonate with controllable topography by using calcium sulfate |
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| CN104046119B (en) * | 2014-07-04 | 2016-03-23 | 成都新柯力化工科技有限公司 | A kind of building coating porous calcium carbonate and preparation method thereof |
| CN104250020B (en) * | 2014-09-24 | 2015-11-04 | 武汉理工大学 | A kind of micro-nano hierarchy of vaterite-type calcium carbonate and additive-free preparation method thereof |
| CN104891548B (en) * | 2015-06-26 | 2016-04-13 | 黑龙江大学 | A kind of preparation method of spherical calcite type calcium carbonate |
| CN108502910B (en) * | 2018-03-01 | 2021-04-30 | 复旦大学 | Insoluble inorganic salt micro-nano material and preparation method and application thereof |
| CN114291836B (en) * | 2021-12-31 | 2023-09-19 | 连州市凯恩斯纳米材料有限公司 | Calcium carbonate crystal form control agent, application thereof and preparation method of cubic calcium carbonate |
| CN114560486B (en) * | 2022-03-03 | 2024-02-27 | 兰州理工大学 | CO with leaching aid capable of being recycled 2 Indirect mineralization method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101045544A (en) * | 2007-04-26 | 2007-10-03 | 安徽工业大学 | Method for preparing superthin light calcium carbonate using plaster as raw material |
| CN101486481A (en) * | 2009-03-02 | 2009-07-22 | 多氟多化工股份有限公司 | Method for coproduction of ammonia sulfate and superfine light calcium carbonate from fluorgypsum |
| CN101830494A (en) * | 2010-05-11 | 2010-09-15 | 安徽工业大学 | Method for preparing active calcium carbonate by taking gypsum as raw material |
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| JP4034982B2 (en) * | 2002-03-29 | 2008-01-16 | 日鉄鉱業株式会社 | Calcium carbonate production method, flue gas desulfurization method or sulfuric acid neutralization method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101045544A (en) * | 2007-04-26 | 2007-10-03 | 安徽工业大学 | Method for preparing superthin light calcium carbonate using plaster as raw material |
| CN101486481A (en) * | 2009-03-02 | 2009-07-22 | 多氟多化工股份有限公司 | Method for coproduction of ammonia sulfate and superfine light calcium carbonate from fluorgypsum |
| CN101830494A (en) * | 2010-05-11 | 2010-09-15 | 安徽工业大学 | Method for preparing active calcium carbonate by taking gypsum as raw material |
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| JP特开2003-292321A 2003.10.15 |
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