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Crystal modifier, medical flaky alpha-hemihydrate calcium sulfate and preparation method thereof

A technology of calcium sulfate hemihydrate and crystallizing agent, which is used in the preparation of sulfide, calcium/strontium/barium sulfate, organic chemistry, etc., can solve problems such as non-conformity, excessive particle size, etc., and achieves convenient operation and particle size. Small, low energy consumption

Active Publication Date: 2019-11-08
HUBEI UNIV FOR NATITIES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the diameter of the flaky α-calcium sulfate hemihydrate crystals is 35-42 μm, which is too large and does not meet the requirements of medical implant bone repair materials.

Method used

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  • Crystal modifier, medical flaky alpha-hemihydrate calcium sulfate and preparation method thereof
  • Crystal modifier, medical flaky alpha-hemihydrate calcium sulfate and preparation method thereof
  • Crystal modifier, medical flaky alpha-hemihydrate calcium sulfate and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] The preparation method of crystal transformation agent:

[0029] Add trihydroxymethylpropane tris(3-mercaptopropionate) (4.0g, 10.0mmol), maleic anhydride (2.94g, 30mmol) and potassium hydroxide 0.15g in 100ml solvent benzene, stir well, heat at 85 Reaction at ℃ for 7.5h. After the reaction, add 20ml of water, adjust the pH to weak acidity, cool and crystallize, suction filter, wash, and dry to obtain white solid trihydroxymethylpropane tris(3-mercaptopropionate)maleic acid.

[0030] Performance Characterization:

[0031] The product was characterized by infrared spectroscopy, IR (KBr) υ: 3267 (-COOH), 2874 (-CH 2 ), 1740(-C=O), 1211(C-O)cm -1 . It was verified that the obtained product was trimethylolpropane tris(3-mercaptopropionate) maleic acid.

Embodiment 2

[0033] The preparation method of medical flake α-calcium sulfate hemihydrate:

[0034] Prepare high-grade pure calcium nitrate solution (1.5mol / L) and potassium sulfate solution (1.5mol / L) respectively, and mix according to the molar mass ratio of calcium nitrate and potassium sulfate of 2.5:1. Then add 2% trihydroxymethylpropane tris(3-mercaptopropionate)maleic acid crystal conversion agent with the total mass of calcium nitrate and potassium sulfate, stir evenly, adjust pH to 5.5, and obtain white slurry. Put the configured slurry in the reactor, heat it, stir and reflux at 95°C for 3 hours, and fully complete the hydrothermal reaction to generate α-calcium sulfate hemihydrate. Suction filter the α-calcium sulfate hemihydrate slurry, wash twice with 95% ethanol, and dry in a constant temperature drying oven at 60°C for 2.0 hours to obtain medical grade flake α-calcium sulfate hemihydrate.

[0035] Performance Characterization:

[0036] Such as figure 1 As shown, the α-cal...

Embodiment 3

[0038] Preparation:

[0039] Prepare high-grade pure calcium nitrate solution (1.5mol / L) and potassium sulfate solution (1.5mol / L) respectively, and mix them according to the molar mass ratio of calcium nitrate and potassium sulfate at a ratio of 3:1. Then add a trihydroxymethylpropane tris(3-mercaptopropionate)maleic acid crystal conversion agent with a total mass of 1.5% of calcium nitrate and potassium sulfate, stir evenly, and adjust the pH to 6.0 to obtain a white slurry. Put the configured slurry in the reactor, heat, stir and reflux at 98°C for 3 hours, fully complete the hydrothermal reaction to generate α-calcium sulfate hemihydrate. Suction filter the α-calcium sulfate hemihydrate slurry, wash twice with 95% ethanol, and dry in a constant temperature drying oven at 60°C for 2.0 hours to obtain medical grade flake α-calcium sulfate hemihydrate.

[0040] Performance Characterization:

[0041] The α-calcium sulfate hemihydrate crystals prepared in Example 3 are flaky,...

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Abstract

The invention provides a crystal modifier, medical flaky alpha-hemihydrate calcium sulfate and a preparation method thereof. The preparation method of the medical flaky alpha-hemihydrate calcium sulfate comprises the following steps: step 1, respectively preparing a calcium salt solution and a sulfate solution, mixing the calcium salt solution and the sulfate solution according to the molar mass ratio of calcium salt to sulfate of 2.5-4:1, adding a trihydroxymethyl propane tris (3-mercaptopropionic acid ester) maleic acid crystal modifier, uniformly stirring, and adjusting pH to 5.5-6.5 to obtain white slurry; step 2, fully stirring and refluxing the prepared slurry in a reactor at 90-100 DEG C to obtain alpha-hemihydrate calcium sulfate slurry; and step 3, performing suction filtering, washing and drying on the slurry. The method can prepare flaky alpha-calcium sulfate hemihydrate crystals with high purity, small particle size and uniform distribution, which meet the requirements of medical implant bone repair materials. The diameter of the flaky alpha-calcium sulfate hemihydrate crystals is less than 5 mu m, the aspect ratio is less than 0.5, the maximum bending strength is as high as 21.4 MPa, and the compressive strength is as high as 50.7 MPa.

Description

technical field [0001] The invention belongs to the field of preparation of α-calcium sulfate hemihydrate, and in particular relates to a small-diameter medical flaky α-calcium sulfate hemihydrate and a preparation method thereof, and a crystal modifier for preparing the medical flaky α-calcium sulfate hemihydrate. [0002] technical background [0003] Calcium sulfate has become a hotspot of artificial bone repair materials due to its good biocompatibility, osteoconductivity and degradability and many other advantages. At present, medical calcium sulfate is usually medical α-calcium sulfate hemihydrate made by a special method. Studies have shown that the comprehensive performance of α-calcium sulfate hemihydrate is closely related to the morphology of crystals. Clinically, only the uniform hexagonal short columnar or hexagonal flaky α-calcium sulfate hemihydrate with high purity and small particle size has good comprehensive performance. performance (patent CN103723757A). ...

Claims

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Application Information

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IPC IPC(8): C01F11/46C07C323/52C07C319/18
CPCC01F11/46C07C323/52C07C319/18C01P2004/03C01P2002/72C01P2004/61
Inventor 冯驸胡超胡颖胡盛胡卫兵余爱农熊枝敏马磊李杨陈盼
Owner HUBEI UNIV FOR NATITIES
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