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Preparation method of calcium carbonate whiskers with concave and convex surface morphology

A technology of calcium carbonate whiskers and concave-convex surface, which is applied in the field of calcium carbonate whiskers to achieve the effects of ensuring purity, enhancing binding ability and large specific surface area

Active Publication Date: 2016-08-31
SHAANXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The technical problem to be solved by the present invention is to overcome the shortcomings of the existing methods for artificially synthesizing calcium carbonate whiskers, and provide a method for preparing calcium carbonate whiskers with special surface morphology by using highly active organic metal calcium sources instead of inorganic calcium salts

Method used

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  • Preparation method of calcium carbonate whiskers with concave and convex surface morphology
  • Preparation method of calcium carbonate whiskers with concave and convex surface morphology
  • Preparation method of calcium carbonate whiskers with concave and convex surface morphology

Examples

Experimental program
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Embodiment 1

[0026] 1. Preparation of calcium precursor solution

[0027] Add 0.204g (2mmol) of newly prepared calcium methoxide with a purity of more than 99% into a 250mL three-necked flask, and add 100mL of anhydrous methanol, and ultrasonically disperse evenly to obtain a calcium methoxide suspension; 0.0114g magnesium ethylate (0.1 mmol) was added to 100mL deionized water to obtain an aqueous solution of magnesium ethoxide; the resulting calcium methoxide suspension was heated to 70-80°C in an oil bath, and was poured into it at a rate of 1 drop / second with a constant pressure funnel under stirring conditions. The obtained magnesium ethoxide aqueous solution was added dropwise. After the dropwise addition, a calcium precursor solution was obtained. The concentration of calcium ions in the obtained calcium precursor solution was 0.02 mol / L, and the concentration of magnesium ions was 0.001 mol / L.

[0028] 2. Preparation of chitosan template

[0029] 2g chitosan is dissolved in 98g mas...

Embodiment 2

[0033] In step 1 of Example 1, 0.102 g (1 mmol) of newly prepared calcium methoxide with a purity of more than 99% was added to a 250 mL three-necked flask, and 100 mL of anhydrous methanol was added, and the ultrasonic dispersion was uniform to obtain calcium methoxide suspension solution; add 0.0114g magnesium ethoxide (0.1mmol) into 100mL deionized water to obtain an aqueous solution of magnesium ethoxide; heat the obtained calcium methoxide suspension to 70-80°C with an oil bath, and use a constant pressure funnel under stirring conditions Add the obtained magnesium ethylate aqueous solution dropwise thereto at a speed of 1 drop / second. After the dropwise addition, a calcium precursor solution is obtained. The concentration of calcium ions in the obtained calcium precursor solution is 0.01mol / L, and the concentration of magnesium ions is 0.001mol / L. . Other steps are identical with embodiment 1, obtain the calcium carbonate whisker with concave-convex surface morphology (s...

Embodiment 3

[0035] In step 1 of Example 1, 0.255 g (2.5 mmol) of newly prepared calcium methoxide with a purity of more than 99% was added to a 250 mL three-necked flask, and 100 mL of anhydrous methanol was added, and the ultrasonic dispersion was uniform to obtain calcium methoxide suspension Turbid liquid; add 0.0114g magnesium ethoxide (0.1mmol) into 100mL deionized water to obtain an aqueous solution of magnesium ethoxide; heat the obtained calcium methoxide suspension to 70-80°C with an oil bath, and use constant pressure to The funnel drips the obtained magnesium ethylate aqueous solution therein at a speed of 1 drop / second. After the dropwise addition, a calcium precursor solution is obtained. The concentration of calcium ions in the gained calcium precursor solution is 0.025mol / L, and the concentration of magnesium ions is 0.001mol / L. L. Other steps are identical with embodiment 1, obtain the calcium carbonate whisker with concave-convex surface morphology (see Figure 4 ), the ...

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Abstract

The invention discloses a preparation method of calcium carbonate whiskers with concave and convex surface morphology. The method is characterized in that organic calcium is used as a calcium source, organic magnesium is a crystal regulating agent, and chitosan is used as a template agent; the mole ratio of calcium ions in the organic calcium to magnesium ions in the organic magnesium is regulated and controlled; meanwhile, carbon dioxide atmosphere is provided through natural decomposition of ammonium carbonate under the sealing condition, so that aragonite type calcium carbonate whiskers (the length diameter ratio is 2 to 20) with regular morphology, the length being 1 to 3mum and the radial length being 0.15 to 0.6mum are obtained. The method has the advantages that the organic calcium and the organic magnesium are used as raw materials; the C1- introduced by common inorganic salts (CaCl2 and MgCl2) is avoided; the purity of the calcium carbonate whisker product is effectively ensured. The surface of the calcium carbonate whiskers prepared by the method is in a granular accumulation morphology; the large specific surface area and the special concave and convex microtopography are realized; the bonding capability with organic matters can be enhanced; other substances are loaded, so that the calcium carbonate whiskers can be used as high-performance polymer composite material fillers and other substance loading substrates.

Description

technical field [0001] The invention belongs to the field of inorganic materials, and specifically relates to a method for synthesizing calcium carbonate whiskers with special concave-convex surfaces by using a highly active organic calcium source to absorb carbon dioxide under the control of organic magnesium. Background technique [0002] Combining the current market and domestic and foreign literature reports, calcium carbonate whiskers can be prepared in the following ways: carbonization method, double decomposition method, urea hydrolysis method, high gravity reaction crystallization method, phosphogypsum hydrothermal synthesis method, and sol-gel method. Among them, both the carbonization method and the double decomposition method need CaCl 2 participation, the introduction of Cl – , when combined with the acidic cations on the surface of cultural relics, it will cause corrosion to stone cultural relics. Although the urea hydrolysis method does not require additional...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/62C30B29/10C30B7/14
CPCC30B7/14C30B29/10C30B29/62
Inventor 金普军柯曾波孙旺罗涛林峰杨国洁
Owner SHAANXI NORMAL UNIV