Hollow calcium carbonate microsphere and preparation method thereof

A hollow microsphere, calcium carbonate technology, applied in the direction of calcium carbonate/strontium/barium, etc., can solve the problems of high additive content, serious product agglomeration, complicated operation, etc., and achieve high biocompatibility and biodegradability. The effect of uniform diameter distribution and simple preparation process

Inactive Publication Date: 2018-06-29
SHANGHAI HUAMING HI TECH GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is cumbersome to operate, and the resulting product is seriously agglomerated and the particle size distribution is uneven.
[0004] In summary, the existing technical solutions have the following disadvantages: one is that the content of hollow microspheres in the product is not high, and the particle size distribution of the microspheres is uneven; the other is that organic solutions or more complex hyperbranched polymer additives are used, And the content of additives is large, the cost is relatively high, and it is not suitable for industrial production
The third is that the reaction time is long and the operation steps are cumbersome, resulting in relatively high preparation cost of calcium carbonate hollow microspheres

Method used

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  • Hollow calcium carbonate microsphere and preparation method thereof
  • Hollow calcium carbonate microsphere and preparation method thereof
  • Hollow calcium carbonate microsphere and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Use water as solvent to prepare 0.1mol / L Na 2 CO 3 solution, 0.1mol / L CaCl 2 solution, 0.5g / L PAA solution (the relative molecular weight of PAA is 2000) and 10.0mmol / L SDS solution. Take out two PAA (each 25mL) solution, add to 100mLNa respectively 2 CO 3 solution and 100mL CaCl 2 Solution, stirred for 0.5h. Add 50mL of SDS solution to the 2 CO 3 and a three-necked flask of a mixed solution of PAA, and then CaCl 2 The mixed solution with PAA was quickly added into the three-necked flask, and the reaction was maintained for 1 hour at 80° C. and a rotation speed of 200 r / min. The resulting CaCO 3 The suspension was filtered, washed three times with deionized water and absolute ethanol, and the filter cake was dried and dehydrated in a drying oven at 80° C. to obtain a white powder product.

[0041] The SEM photo and TEM photo of the product are attached figure 1 And attached figure 2 , the average particle size is 6.2 μm, the molar content of its vaterite ca...

Embodiment 2

[0043] Use water as solvent to prepare 1.0mol / L Na 2 CO 3 Solution, 1.0mol / L CaCl 2 Solution, 1.0g / L PAA solution (the relative molecular weight of PAA is 5000) and 25.0mmol / L SDS solution. Two parts of PAA (each 25mL) solution were taken out and added to 100mL Na 2 CO 3 solution and 100mL CaCl 2 solution, 0.5h. Add 50mL of SDS solution to the 2 CO 3 and a three-necked flask of a mixed solution of PAA, and then CaCl 2 The mixed solution with PAA was quickly added into the three-necked flask, and the reaction was maintained for 1 hour at 90°C and the rotation speed was 200r / min. The resulting CaCO 3 The suspension was filtered, washed three times with deionized water and absolute ethanol, and the filter cake was dried and dehydrated in a drying oven at 80° C. to obtain a white powdery product.

[0044] The SEM photo of the product is attached image 3 , with an average particle size of 6.8 μm, see the attached XRD pattern Figure 4 , the molar content of vaterite ca...

Embodiment 3

[0046] According to the same method as in Example 1, the difference is: Na 2 CO 3 The solution concentration is 0.5mol / L; CaCl 2 The solution concentration is 0.5mol / L; the molecular weight of PAA is 3000, and its concentration is 0.8g / L; the concentration of SDS is 15.0mmol / L; the reaction temperature is 60°C.

[0047] The SEM photo of the product is attached Figure 5 , with an average particle size of 5.2 μm, see the attached XRD pattern Figure 6 , its vaterite calcium carbonate molar content is 46.8% (calcite calcium carbonate molar content is 53.2%), and its specific surface area is 40.6m 2 / g, and the average pore diameter is 18.49nm, showing that the product is a calcium carbonate hollow microsphere with a large specific surface area. Other test and calculation data are shown in Table 1.

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Abstract

The invention discloses a hollow calcium carbonate microsphere and a preparation method thereof. The preparation method comprises the following steps: 1, preparing solutions of calcium chloride (CaCl2), sodium carbonate (Na2CO3), polyacrylic acid (PAA) and sodium dodecyl sulfate (SDS); 2, adding the prepared PAA in constant volume into the Na2CO3 solution and the CaCl2 solution; 3, adding the SDSsolution into a mixed solution containing the Na2CO3 and PAA only, and adding the solution into a mixed solution of CaCl2 and PAA; 4, filtering, washing and drying the reaction product, thereby obtaining the white powdered hollow calcium carbonate microsphere with excellent monodispersity. The obtained hollow calcium carbonate microsphere has a compound crystal form of calcite and vaterite, is uniform in particle size distribution, does not have an agglomeration phenomenon, and has the mean grain size of 5-8 microns and the specific surface area of 30-60m<2> / g. The preparation method is simplein process, low in cost, easy to control, green, environmentally friendly and capable of realizing industrialized production; the prepared hollow calcium carbonate microsphere has huge application value in the fields of drug sustained release and the like.

Description

technical field [0001] The invention relates to a preparation method of calcium carbonate hollow microspheres containing vaterite and calcite crystal forms, which belongs to the field of inorganic powder materials, can be applied to fillers of building materials, plastics, inks, rubber, etc., and has high biocompatibility And biodegradability, can be used as biomedicine and new drug carrier. Background technique [0002] Calcium carbonate is an important inorganic material and a typical biomineral, widely used in plastics, paper, ink, paint, textile, adhesive, cosmetics, food and other industries. In nature, calcium carbonate mainly has three different crystal forms: calcite, aragonite and vaterite, among which calcite is the most stable crystal form in thermodynamics, followed by aragonite, and vaterite is the most unstable crystal form, which is easy to transform It is thermodynamically stable calcite or aragonite. In terms of appearance structure, calcium carbonate has ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F11/18
CPCC01F11/18C01P2002/72C01P2004/03C01P2004/04C01P2004/61C01P2006/12C01P2006/14C01P2006/16
Inventor 陈雪梅郑天文程鏖
Owner SHANGHAI HUAMING HI TECH GRP
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