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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 crystallization of calcium carbonate. The crystalline form and particle size of calcium overcome the problems of wide particle size distribution and poor crystal form stability (easy to convert into thermodynamically stable calcite crystal form in mother liquor or humid environment) and other problems in the current invention

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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Effect test

Embodiment 1

[0048] (1) Preparation of carboxyl-functionalized hyperbranched polyglycidyl ether: weigh 1.48mmol in a dry three-necked bottle, and the degree of polymerization is 21 hydroxyl hyperbranched polyglycidyl ether, dissolve with 30mL dimethylacetamide, Add 35.5mmol of succinic anhydride and 0.01g of 4-dimethylaminopyridine, heat to 100°C under nitrogen protection and stir for 6h; cool to room temperature, add 15mL of methanol, and stir for 12h; Drop into the mixed solvent of dichloromethane / diethyl ether (volume ratio is 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; Concentrate and dry to obtain carboxyl functionalized hyperbranched polyglycidyl ether (molecular structure schematic diagram as figure 1 ), productive rate 89%; Characterization result is as follows: 1 H NMR (Acetone-d 6 , 300MHz): (ppm) 0.78 (m, -CH 2 C ...

Embodiment 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: 150 mg / L): Add 75 mg of carboxyl-functionalized hyperbranched polyglycidyl ether solid into 500 mL of deionized water, stir until completely dissolved, and use hydrogen oxidation Sodium or hydrochloric acid adjustment solution pH value is 10;

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

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

Embodiment 3

[0060] (1) Preparation of carboxyl functionalized hyperbranched polyglycidyl ether: weigh 0.72mmol in a dry three-neck bottle, and the degree of polymerization is 45 hydroxyl hyperbranched polyglycidyl ether, dissolve with 40mL dimethylacetamide, Add 38.1 mmol of succinic anhydride and 0.02 g of 4-dimethylaminopyridine, heat to 100°C under nitrogen protection and stir for 6 h; cool to room temperature, add 15 mL of methanol, and stir for 12 h; the obtained reaction solution is firstly distilled off under reduced pressure to remove methanol; Then drop into the mixed solvent of dichloromethane / ether (volume ratio is 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 48h to remove small molecules and ion impurities; finally Carboxyl functionalized hyperbranched polyglycidyl ether can be obtained after concentration and drying with a yield of 85%; the characterization results are as ...

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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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