CN103395812A - Method for controlling shape of calcium carbonate in solid carbonization process - Google Patents
Method for controlling shape of calcium carbonate in solid carbonization process Download PDFInfo
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- CN103395812A CN103395812A CN2013102924279A CN201310292427A CN103395812A CN 103395812 A CN103395812 A CN 103395812A CN 2013102924279 A CN2013102924279 A CN 2013102924279A CN 201310292427 A CN201310292427 A CN 201310292427A CN 103395812 A CN103395812 A CN 103395812A
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- calcium carbonate
- cyclodextrin
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Abstract
The invention belongs to the technical field of preparation of calcium carbonate, and relates to a method for controlling shape of calcium carbonate in a solid carbonization process. The method comprises the following steps: mixing calcium hydroxide, beta-cyclodextrin and water in a ratio of 100:(3-10):(5-15), carrying out compression molding under the pressure of 2.0-15.0 MPa, and carbonizing in a closed reaction kettle, wherein the carbonization conditions are as follows: the CO2 gas pressure is 0.1-0.6 MPa, the reaction kettle temperature is 25-55 DEG C, the humidity is 65-80%, and the carbonization time is 4-12 hours. The invention introduces the method of controlling the shape of the calcium carbonate crystal by utilizing polysaccharide in a liquid into the solid carbonization. The beta-cyclodextrin can enhance the compression strength of the carbonized test block and improve the carbonization efficiency, so that the shape of the carbonization product is greatly changed. In the solid carbonization process, the control of the shape of the calcium carbonate crystal by beta-cyclodextrin is completely feasible.
Description
Technical field
The invention belongs to the calcium carbonate preparing technical field, relate to a kind of polysaccharide macro-molecular that utilizes and control the method that generates the calcium carbonate product pattern in the solid carbonization.
Background technology
Calcium carbonate is the modal mineral of a kind of occurring in nature, mainly with six kinds of forms, exists: calcite, aragonite, vaterite and three kinds of amorphous calcium carbonates.Calcium carbonate is widely used in the industries such as papermaking, coating, plastics, medicine, food, building materials, rubber.Different industries has different requirements to its physics, chemical property.In actual production, in rubber, plastics and paper, add the calcium carbonate of appropriate specific morphology can improve well its mechanical property.And along with the scope of calcium carbonate applications is more and more wider, the Aragonite Style Calcium Carbonate Whiskers with needle bar shape pattern also well is applied in cement-based material.
Beta-cyclodextrin has the ring shaped molecule structure shown in figure below:
At home, the people such as Zhang Hui is at CaCl
2With NaCO
3In mixing solutions, utilize beta-cyclodextrin to control and generated take vaterite as main CaCO
3The stratiform aggregate, and the people such as Zhang Xiuying are usingd beta-cyclodextrin as the bionical CaCO that consists of the deer horn shape nanocluster of growing thickly that synthesized of organic substrate
3Crystal.Pertinent literature as:
[document 1] Zhang Hui, Yin Xiaoshuan, Yang Wenzhong. chain and cyclic polysaccharide regulation and control CaCO
3Bionical synthetic [J]. Nanjing University of Technology's journal (natural science edition), 2010,32 (1): 50-54;
[document 2] Zhang Xiuying, Liao Zhaojiang, Yang Lin. the interaction of beta-cyclodextrin and calcium carbonate crystal [J]. chemical journal, 2003,61 (1): 69-73;
Abroad, Venous Derakhshanian and Sujit Banerjee also utilize beta-cyclodextrin to suppress the growth of calcium carbonate crystal, reduce to generate the size of calcium carbonate.Detailed content referring to:
[document 3] Venous Derakhshanian, Sujit Banerjee.Cyclodextrin Inhibits Calcium Carbonate Crystallization and Scaling[J] .Industrial & Engineering Chemistry Research, 2012,51,4463-4465.
Yet above achievement in research is all to carry out in liquid reaction system, and use be chemical synthesis.
In recent years, problem of environmental pollution more and more receives people's concern, and has become two hang-ups of curbing environmental pollution as the two large sources (waste gas and waste residue) of polluting.Through lot of experiments research, the solid carbon of mineral becomes a kind of method that can the permanent storage carbonic acid gas.The solid carbon of mineral not only can adsorb the carbonic acid gas in atmosphere, but also can prepare building material made by the carbonization to mineral, reaches the effect of killing two birds with one stone.
The composition that can be carbonized in waste cement and abandoned mine slag mainly comprises: calcium oxide, calcium hydroxide, Dicalcium Phosphate (Feed Grade), tricalcium silicate, hydrated calcium silicate, drated calcium aluminate, hydrated calcium ferrite, ettringite, magnesium hydroxide and magnesium oxide etc., and the carburizing reagent of generation is as follows:
Ca(OH)
2+CO
2→CaCO
3
CaO+CO
2→CaCO
3
MgO+CO
2→MgCO
3
3CaO·SiO
2+3CO
2+μH
2O→SiO
2·μH
2O+3CaCO
3
2CaO·SiO
2+2CO
2+μH
2O→SiO
2·μH
2O+2CaCO
3
Along with people deepen continuously to the research of the solid carbon of mineral and waste recycling, the application of solid carborization has become focus.This be due to, but utilize carbonation method to prepare building material made, not only to improve carbonization efficiency to take full advantage of the carbonization elements in discarded mineral as far as possible; And to make carbonization product have the intensity that meets service requirements.This two aspect must be achieved in solid state reaction.And the pattern of carbonized product calcium carbonate crystal is remarkable on the macro properties such as the intensity impact of goods.Therefore, be necessary very much to attempt controlling the pattern of calcium carbonate crystal in the solid phase carbonization process.
Summary of the invention
The present invention utilizes beta-cyclodextrin (C
6H
10O
5)
nXH
2O controls the pattern of calcium hydroxide carbonization generation calcium carbonate in the solid carborization.Under condition of the present invention, can generate the calcium carbonate of the hollow tubular pattern that is similar to the beta-cyclodextrin molecular structure.
Technical scheme of the present invention is as follows:
A kind of method of controlling shape and appearance of calcium carbonate in the solid carborization, raw material is calcium hydroxide, beta-cyclodextrin and water, carburizing reagent, through 2.0～15.0MPa pressure forming, occur in calcium hydroxide: beta-cyclodextrin: water=100:3～10:5～15 in closed reactor.
Carbonization Conditions of the present invention is: CO
2Air pressure 0.1～0.6MPa; 25～55 ℃ of reactor temperatures, humidity 65～80%, carbonization time 4～12h.
The present invention will utilize polysaccharide to control the calcium carbonate crystal pattern in liquid method is incorporated in the solid carbonization.Beta-cyclodextrin not only can improve test block pressure resistance intensity after carbonization, and can also improve carbonization efficiency, and the pattern of carbonized product has produced very large change.Verified in the solid carbonization, utilized beta-cyclodextrin to control the calcium carbonate crystal pattern feasible.
The accompanying drawing explanation
Fig. 1 is sample micro-structure diagram after the embodiment carbonization.
Fig. 2 is sample XRD figure after the embodiment carbonization.
In figure: ★ represents the diffractive features peak of calcium hydroxide, ◆ the diffractive features peak of expression calcite type calcium carbonate.
Embodiment
Embodiment 1:
Adopt calcium hydroxide: beta-cyclodextrin: water=100:4:10, through the 5MPa pressure forming, carry out carbonization in closed reactor.Carbonization Conditions is: CO
2Air pressure 0.2MPa; 30 ℃ of temperature of reaction kettle, humidity 70%, carbonization time 4h.
Embodiment 2:
Adopt calcium hydroxide: beta-cyclodextrin: water=100:6:8, through the 8MPa pressure forming, carry out carbonization in closed reactor.Carbonization Conditions is: CO
2Air pressure 0.2MPa; 35 ℃ of temperature of reaction kettle, humidity 65%, carbonization time 6h.
Embodiment 3:
Adopt calcium hydroxide: beta-cyclodextrin: water=100:6:15, through the 12MPa pressure forming, carry out carbonization in closed reactor.Carbonization Conditions is: CO
2Air pressure 0.5MPa; 40 ℃ of temperature of reaction kettle, humidity 80%, carbonization time 12h.
Test case
X-ray diffraction (XRD) and scanning electronic microscope (SEM) test are done in sampling in the embodiment dry sample, and the conclusion that draws such as Fig. 1, shown in 2.XRD result in Fig. 2 shows that the carbonized product crystal formation is calcite type calcium carbonate; The SEM picture can find out, the calcium carbonate microscopic appearance is the hollow annular structure.
Claims (2)
1. method of controlling shape and appearance of calcium carbonate in the solid carborization, it is characterized in that, raw material is calcium hydroxide, beta-cyclodextrin and water, calcium hydroxide: beta-cyclodextrin: water=100:3～10:5～15, through 2.0～15.0MPa pressure forming, carburizing reagent occurs in closed reactor.
2. method according to claim 1, is characterized in that, Carbonization Conditions is: CO
2Air pressure 0.1～0.6MPa; 25～55 ℃ of temperature of reaction kettle, humidity 65～80%, carbonization time 4～12h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115897285A (en) * | 2023-01-03 | 2023-04-04 | 北京化工大学 | Transparent nano calcium carbonate aqueous phase dispersion and preparation method thereof |
Citations (9)
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| US5332564A (en) * | 1992-07-10 | 1994-07-26 | Ecc International Inc. | Process for production of rhombic shaped precipitated calcium carbonate |
| EP0459399B1 (en) * | 1990-05-28 | 1994-08-17 | Maruo Calcium Company Limited | Monodisperse vaterite type calcium carbonate, its manufacturing method and method of controlling growth of particles and shape thereof |
| CN1169955A (en) * | 1996-05-03 | 1998-01-14 | 俞圭在 | Process for producing calcium carbonate particles having size of 0.1 to 1.0 micrometer |
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| CN101108741A (en) * | 2006-07-21 | 2008-01-23 | 北京市化工建材厂 | Industrial process for preparing nm-class active calcium carbonate |
| CN102491396A (en) * | 2011-11-30 | 2012-06-13 | 厦门大学 | Method for preparing nanometer calcium carbonate |
-
2013
- 2013-07-11 CN CN201310292427.9A patent/CN103395812B/en active Active
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|---|---|---|---|---|
| GB1239407A (en) * | 1967-09-25 | 1971-07-14 | ||
| EP0459399B1 (en) * | 1990-05-28 | 1994-08-17 | Maruo Calcium Company Limited | Monodisperse vaterite type calcium carbonate, its manufacturing method and method of controlling growth of particles and shape thereof |
| US5332564A (en) * | 1992-07-10 | 1994-07-26 | Ecc International Inc. | Process for production of rhombic shaped precipitated calcium carbonate |
| CN1169955A (en) * | 1996-05-03 | 1998-01-14 | 俞圭在 | Process for producing calcium carbonate particles having size of 0.1 to 1.0 micrometer |
| CN1348428A (en) * | 1999-03-31 | 2002-05-08 | 矿业技术有限公司 | Process for the preparation of discrete particles of calcium carbonate |
| CN101108741A (en) * | 2006-07-21 | 2008-01-23 | 北京市化工建材厂 | Industrial process for preparing nm-class active calcium carbonate |
| CN101037214A (en) * | 2007-03-23 | 2007-09-19 | 上海耀华纳米科技有限公司 | Preparation method of novel nano calcium carbonate |
| CN101037215A (en) * | 2007-03-23 | 2007-09-19 | 上海耀华纳米科技有限公司 | Preparation process of light calcium carbonate serosity |
| CN102491396A (en) * | 2011-11-30 | 2012-06-13 | 厦门大学 | Method for preparing nanometer calcium carbonate |
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| Title |
|---|
| 常钧等: "用碳化养护电弧熔炉钢渣制备集料和混凝土", 《硅酸盐学报》, vol. 35, no. 9, 30 September 2007 (2007-09-30), pages 1264 - 1269 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115897285A (en) * | 2023-01-03 | 2023-04-04 | 北京化工大学 | Transparent nano calcium carbonate aqueous phase dispersion and preparation method thereof |
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