Monodispersed vaterite type calcium carbonate microsphere and preparation method thereof

A technology of calcium carbonate and vaterite, applied in the direction of calcium carbonate/strontium/barium, etc., can solve the problems of wide particle size distribution and poor crystal stability, and achieve high density of surface functional groups, low cost and short aging time. Effect

Inactive Publication Date: 2012-07-18
NANJING UNIVERSTIY SUZHOU HIGH TECH INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Studies have shown that macromolecular crystallization modifiers with special functional groups and specific molecular secondary structures are highly selective to the crystal phase of calcium carbonate (Journal of the American Chemical Society, 2002, 124: 9700-9701), which can effectively regulate the crystallizat

Method used

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  • Monodispersed vaterite type calcium carbonate microsphere and preparation method thereof
  • Monodispersed vaterite type calcium carbonate microsphere and preparation method thereof
  • Monodispersed vaterite type calcium carbonate microsphere and preparation method thereof

Examples

Experimental program
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Example Embodiment

[0047] Example 1

[0048] (1) Preparation of carboxyl functionalized hyperbranched polyglycidyl ether: Weigh 1.48mmol of hydroxyl hyperbranched polyglycidyl ether with a degree of polymerization of 21 in a dry three-necked flask and dissolve it with 30mL of dimethylacetamide. Add 35.5mmol succinic anhydride and 0.01g 4-dimethylaminopyridine, heat to 100°C under the protection of nitrogen and stir for 6h; cool to room temperature, add 15mL methanol, and stir for 12h; the resulting reaction solution is first distilled under reduced pressure to remove methanol; Drop into the mixed solvent of dichloromethane / ether (volume ratio 1:2) to precipitate the crude product; then transfer it to a dialysis membrane with a molecular weight cutoff of 500 and dialyze in deionized water for 48 hours to remove small molecules and ionic impurities; Concentrate and dry to obtain hyperbranched polyglycidyl ether functionalized with carboxyl groups (the schematic diagram of the molecular structure is a...

Example Embodiment

[0053] Example 2

[0054] (1) The preparation method of the carboxyl functionalized hyperbranched polyglycidyl ether in this example is the same as in Example 1;

[0055] (2) Preparation of carboxyl functionalized hyperbranched polyglycidyl ether aqueous solution (concentration of 150mg / L): add 75mg of carboxyl functionalized hyperbranched polyglycidyl ether solid into 500mL deionized water, stir until all is dissolved, use hydroxide Adjust the pH of the solution to 10 with sodium or hydrochloric acid;

[0056] (3) Preparation of calcium chloride aqueous solution (concentration of 150mmol / L): Add 8.33g of anhydrous calcium chloride solid to 500mL of deionized water, stir until all is dissolved, use sodium hydroxide or hydrochloric acid to adjust the pH of the solution to 10;

[0057] (4) Preparation of sodium carbonate aqueous solution (concentration of 150mmol / L): add 7.95g of sodium carbonate solid to 500mL of deionized water, stir until all is dissolved, use sodium hydroxide or hyd...

Example Embodiment

[0059] Example 3

[0060] (1) Preparation of carboxyl functionalized hyperbranched polyglycidyl ether: Weigh 0.72mmol of hydroxy hyperbranched polyglycidyl ether with a degree of polymerization of 45 in a dry three-necked flask, and dissolve it with 40mL of dimethylacetamide. Add 38.1mmol of succinic anhydride and 0.02g 4-dimethylaminopyridine, heat to 100°C under the protection of nitrogen, and stir for 6h; cool to room temperature, add 15mL methanol, and stir for 12h; the resulting reaction solution is first distilled under reduced pressure to remove methanol; Then drop into the dichloromethane / ether mixed solvent (volume ratio 1:2) to precipitate the crude product; then transfer to a dialysis membrane with a molecular weight cut-off of 500 and dialyze in deionized water for 48 hours to remove small molecules and ionic impurities; After concentration and drying, the carboxyl functionalized hyperbranched polyglycidyl ether can be obtained with a yield of 85%; the characterizatio...

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Abstract

The invention relates to a preparation method of a monodispersed vaterite type calcium carbonate microsphere, which comprises the following steps of: (1) preparing a calcium salt aqueous solution with the concentration of 30-150mmol/L, and then, adjusting the pH value of the calcium salt aqueous solution to 8.5-10; (2) preparing a carbonate or hydrocarbonate aqueous solution with the concentration of 30-150mmol/L, and then, adjusting the pH value of the carbonate or hydrocarbonate aqueous solution to 8.5-10; (3) preparing a functional hyperbranched polyglycerol aqueous solution with the concentration of 20-400mg/L, and then, adjusting the pH value of the functional hyperbranched polyglycerol aqueous solution to 8.5-10; (4) mixing and uniformly stirring the carbonate or hydrocarbonate aqueous solution, the calcium salt aqueous solution and the functional hyperbranched polyglycerol aqueous solution at the temperature of 10-35 DEG C, and aging for 1-12h; and (5) centrifuging or filtering the mixed solution, cleaning a sediment, and drying to obtain the monodispersed vaterite type calcium carbonate microsphere. The monodispersed vaterite type calcium carbonate microsphere prepared by using the preparation method provided by the invention has the advantages of uniform particle size, stable crystal form and industrial application value.

Description

technical field [0001] The invention relates to a monodisperse vaterite-type calcium carbonate microsphere, and at the same time relates to a method for preparing the calcium carbonate microsphere and its substance by using carboxyl or phosphoric acid functionalized hyperbranched polyglycidyl ether as a crystal regulator. Background technique [0002] Calcium carbonate is a kind of inorganic mineral widely distributed in nature, and it is also widely used as an important chemical filler in many industries such as coatings, inks, rubber, plastics, papermaking and building materials. It has three anhydrous forms: calcite, aragonite and vaterite. Calcite belongs to the triclinic crystal system, and the crystals are rhombic cubes and spindles. It has the highest thermodynamic stability and is the main form of calcium carbonate in geological minerals and industrial applications; aragonite belongs to the orthorhombic crystal system, which is needle-shaped or columnar. It has obvi...

Claims

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Application Information

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IPC IPC(8): C01F11/18
Inventor 谌东中陈钊聪赵辉孟庆伟
Owner NANJING UNIVERSTIY SUZHOU HIGH TECH INST
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