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Organic solvent hydrothermal method for preparing cubic, flower-like or porous calcium carbonate

A technology of porous calcium carbonate and organic solvent, applied in the direction of calcium carbonate/strontium/barium etc.

Inactive Publication Date: 2010-12-29
BEIJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although it has been reported in the literature that oleic acid was used as a solvent to prepare Mn 3 o 4 (J. Seo, et al. The Journal of Physical Chemistry B, 2005, 109: 5389-5381), γ-Fe 2 o 3 (A.L.Willis, et al. Chemistry of Materials, 2005, 17: 5970-5975), FePtAu (S. Kinge, et al. Nano Letters, 2009, 9: 3220-3224), CoFe 2 o 4 (M.V.Limaye, et al. The Journal of Physical Chemistry B, 2009, 113: 9070-9076), NaLa(MoO4) 2 (W.Bu, et al. The Journal of Physical Chemistry C, 2009, 113: 12176-12185) and other nano-metal oxides or composite oxides, but so far no literature and patents have reported the use of organic solvothermal method to prepare calcium carbonate with a specific morphology porous structure

Method used

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  • Organic solvent hydrothermal method for preparing cubic, flower-like or porous calcium carbonate
  • Organic solvent hydrothermal method for preparing cubic, flower-like or porous calcium carbonate

Examples

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Embodiment 1

[0018] Example 1: Get 30mL of oleic acid, put it in a 100mL beaker, add 10mL of dehydrated ethanol (the volume ratio of dehydrated alcohol and oleic acid is 1:3) under magnetic stirring conditions, add 0.84g after stirring for 1h at room temperature Irregular non-porous calcium oxide raw material (that is, the calcium oxide concentration is 0.33mol / L), after continuing to stir for 1h, the solution is transferred to an autoclave with a polytetrafluoroethylene liner with a volume of 50mL (volume filling degree 80 %), kept at 160°C for 6h, and allowed to cool naturally to room temperature after taking it out, the resulting mixture was filtered by suction and washed 3-4 times with absolute ethanol to obtain a white powder, which was stored under the condition of relative humidity of 35-40%. Dry at room temperature. The dried powder is raised from room temperature to 550°C at a rate of 1°C / min in an air atmosphere in a muffle furnace, and kept at this temperature for 3 hours to obt...

Embodiment 2

[0019] Embodiment 2: get 20mL oleic acid, be placed in 100mL beaker, add 2.60g CTAB (that is to control CTAB concentration be 0.42mol / L) under the condition of magnetic stirring, add 20mL dehydrated alcohol after stirring 1h (dehydrated alcohol and oil The volume ratio of the acid is 1:1), after stirring evenly, add 0.75g of irregular non-porous calcium oxide raw material (that is, control the molar ratio of calcium oxide and CTAB to be 8:5), continue stirring for 1h, and transfer the solution to a In a polytetrafluoroethylene-lined autoclave with a volume of 50 mL (filling degree 80 vol%), keep the temperature at 160 ° C for 6 h, take it out and allow it to cool naturally to room temperature, and the resulting mixture is suction filtered and washed with absolute ethanol for 3 - 4 times a white powder was obtained, which was dried at room temperature at a relative humidity of 35-40%. The dried powder is raised from room temperature to 550°C at a rate of 1°C / min in an air atmos...

Embodiment 3

[0020] Embodiment 3: Get 20mL oleic acid, place in 100mL beaker, add 3.85g sodium dodecyl sulfate (SDS, control SDS concentration is 0.67mol / L) under magnetic stirring condition, add 20mL dehydrated alcohol after stirring 1h (The volume ratio of dehydrated alcohol and oleic acid is 1: 1), after stirring evenly, add 0.75g irregular non-porous calcium oxide raw material (that is, control the mol ratio of calcium oxide and SDS to be 8: 8), after continuing to stir for 1h, Transfer the solution to an autoclave with a polytetrafluoroethylene liner with a volume of 50mL (volume filling degree 80%), keep the temperature at 240°C for 6h, let it cool down to room temperature naturally after taking it out, and filter the resulting mixture with suction and washing with absolute ethanol for 3-4 times to obtain a white powder, which is dried at room temperature under the condition of relative humidity of 35-40%. The dried powder is raised from room temperature to 550°C at a rate of 1°C / min...

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Abstract

The invention discloses an organic solvent hydrothermal method for preparing cubic, flower-like or porous calcium carbonate, which comprises: dissolving irregular nonporous calcium oxide raw material in a surfactant-containing / surfactant-free organic mixed solution of absolute ethanol and oleic acid; and treating the mixture in a self-pressurizing kettle, filtering under vacuum, washing, drying and calcining in an early muffle furnace to obtain cubic, flower-like or porous calcium carbonate nano particles, wherein cubic calcium carbonate nano particles are obtained when the mixed solvent does not contain any surfactant, flower-like calcium carbonate nano particles are obtained when the mixed solvent contains a CTAB surfactant, and porous calcium carbonate nano particles are obtained when the mixed solvent contains a PVP or SDS surfactant.

Description

technical field [0001] The invention relates to an organic solvothermal method for preparing calcium carbonate, in particular to a method for preparing cubic, flower-like or porous calcium carbonate by solvothermal method using oleic acid and absolute ethanol as solvents. Background of the invention [0002] Calcium carbonate is widely used in agriculture, papermaking, rubber, plastics, paint and other industrial fields. The practical application of calcium carbonate is related to its properties (such as morphology, particle size, specific surface area, brightness, oil adsorption, etc.). Therefore, it is of great significance to develop controllable preparation methods of calcium carbonate with specific morphology and high specific surface area. [0003] At present, the methods for preparing calcium carbonate with specific morphology mainly include precipitation method, hydrothermal method, hard template method and so on. For example, Lei et al. (M.Lei, et al.Journal of Cr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F11/18
Inventor 戴洪兴赵振璇张汝珍孟雪蒋海燕袁静何洪
Owner BEIJING UNIV OF TECH