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Preparation method of fluorine-containing α-calcium sulfate hemihydrate powder and calcium sulfate artificial bone material

A technology of calcium sulfate hemihydrate and calcium sulfate dihydrate, which is used in dental preparations, dental prostheses, pharmaceutical formulations, etc., to solve the problem of insufficient bone mass, improve bone formation ability, and good biocompatibility.

Active Publication Date: 2016-01-20
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there is no report on the fluorine-containing calcium sulfate hemihydrate material

Method used

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  • Preparation method of fluorine-containing α-calcium sulfate hemihydrate powder and calcium sulfate artificial bone material
  • Preparation method of fluorine-containing α-calcium sulfate hemihydrate powder and calcium sulfate artificial bone material
  • Preparation method of fluorine-containing α-calcium sulfate hemihydrate powder and calcium sulfate artificial bone material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] In this example, basically the same as the comparative example above, the fluorine-containing α-calcium sulfate hemihydrate powder is prepared by dehydration reaction of calcium sulfate dihydrate in a mixed reaction solution of calcium chloride aqueous solution and absolute ethanol. The difference is that ammonium fluoride is added as a fluorinating agent in the mixed reaction solution. Wherein, the mass ratio that calcium chloride accounts for distilled water is 0.3, and the volume ratio of dehydrated alcohol and distilled water is 1, and the mass ratio of calcium sulfate dihydrate and mixed reaction solution is 0.0355, and the mol ratio of ammonium fluoride and calcium sulfate dihydrate is 0.005.

[0048] The concrete preparation method of this fluorine-containing α-calcium sulfate hemihydrate powder comprises the steps:

[0049] (1) At room temperature, add 0.00645g of ammonium fluoride to 210ml of distilled water for ultrasonic dispersion for 5 minutes, then add 90...

Embodiment 2

[0059] In this embodiment, it is basically the same as the above-mentioned embodiment 1. The fluorine-containing α-calcium sulfate hemihydrate powder is prepared by the dehydration reaction of calcium sulfate dihydrate in a mixed reaction solution of calcium chloride aqueous solution, absolute ethanol and ammonium fluoride. have to. The difference is that the amount of ammonium fluoride added is different, and the molar ratio of ammonium fluoride to calcium sulfate dihydrate is 0.01.

[0060] The concrete preparation method of this α-calcium sulfate hemihydrate powder comprises the steps:

[0061] (1) At room temperature, add 0.0129g of ammonium fluoride to 210ml of distilled water for ultrasonic dispersion for 5 minutes, then add 90g of anhydrous calcium chloride, stir for 10 minutes to completely dissolve, continue to add 175ml of absolute ethanol, and stir for 30 minutes After obtaining a uniform mixed reaction solution;

[0062] (2) Pour the reaction liquid obtained in s...

Embodiment 3～6

[0071] In the following examples 3 to 6, it is basically the same as the above-mentioned comparative example. The fluorine-containing α-calcium sulfate hemihydrate powder is composed of calcium sulfate dihydrate in calcium chloride aqueous solution, dehydrated alcohol and mixed reaction solution with ammonium fluoride The reaction conditions are the same as those in Example 1, except for the amount of ammonium fluoride added (see Table 1 below for details).

[0072] Ammonium fluoride addition (relative to the mol ratio of calcium sulfate dihydrate) in table 1 embodiment 3~6

[0073] Example

Amount of ammonium fluoride added

3

0.02

4

0.03

5

0.05

6

0.07

[0074] The phase of the fluorine-containing α-calcium sulfate hemihydrate powder obtained above is analyzed, and similar figure 1 As shown in the XRD spectrum, the obtained powder is highly pure α-calcium sulfate hemihydrate, without calcium sulfate dihydrate resi...

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Abstract

The invention discloses preparation methods for fluorine-containing alpha-calcium sulfate hemihydrate powder and a fluorine-containing calcium sulfate artificial bone material, and belongs to the field of medical biological materials. The preparation method for the fluorine-containing alpha-calcium sulfate hemihydrate powder is as follows: adding a fluorinating agent in a process of adding calcium sulfate dihydrate into mixed reaction liquor of calcium chloride aqueous liquor and absolute ethyl alcohol for partly removing crystalline water to prepare alpha-calcium sulfate hemihydrate, so that fluoride ions partly substitute ions in calcium sulfate hemihydrate to prepare the fluorine-containing alpha-calcium sulfate hemihydrate powder. The fluoride ions change crystal structure of calcium sulfate hemihydrate, so that the crystalline grain feature of the fluorine-containing alpha-calcium sulfate hemihydrate powder is obviously changed to an equiaxial hexagonal prism shape from a slender prism shape. The material has good degradation property and biocompatibility, and therefore, the prepared fluorine-containing alpha-calcium sulfate hemihydrate artificial bone material can be applied to the medical repair field, for example, can be used as dental materials such as a dental cementation material, dental filler, a pit and fissure sealant, and the like, and can be used as a root canal product, and the like.

Description

technical field [0001] The present invention relates to a preparation method of a novel self-curing calcium sulfate material, and its application as a bone graft substitute material in dental implant surgery, such as dental cement material, dental filling, pit and fissure sealant, and For root canal products, etc. Background technique [0002] Calcium sulfate has been widely recognized as a bone graft substitute material and guided tissue regeneration material because of its good biocompatibility, biodegradation, non-toxicity, good hemostasis and angiogenesis, and osteoconduction and osteoinduction. use. [0003] Calcium sulfate hemihydrate is calcium sulfate dihydrate to remove 1.5H 2 Formed after O, upon rehydration (i.e. binding of 1.5H per molecule of calcium sulfate hemihydrate 2 O) become calcium sulfate dihydrate again. Calcium sulfate hemihydrate has strong plasticity and self-curing in situ, and can be made into various shapes according to the conditions of bone...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): A61K6/027
Inventor 刘建莉黄庆徐华梓彭磊潘宗友杨光永
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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