Preparation method of high-purity surgical grade alpha-calcium sulfate hemihydrate with adjustable crystal size

Abstract

The invention discloses a preparation method of high-purity surgical-grade alpha-hemihydrate sulfuric acid with adjustable crystal size, and belongs to the field of medical biological materials. By adjusting the mass ratio of the mixed crystal modifier to the deionized water, the size (10-60 m) of the alpha-calcium sulfate hemihydrate crystal is effectively regulated, the length-diameter ratio is (1-5): 1, and the uniformly distributed crystal alpha-calcium sulfate hemihydrate powder is obtained. And the infrared spectrum curve of the calcium sulfate hemihydrate crystal has the characteristics that the H2O characteristic peak intensity at 1622 cm <-1 > and the O-H characteristic peak intensity and width at 3612 cm <-1 > and 3559 cm <-1 > are reduced along with the reduction of the particle size. After the calcium sulfate hemihydrate is mixed and cured with a curing liquid, the compressive strength is 25-35 MPa, so that the requirements of different load bearing parts on the mechanical strength are met. The degradation time is 60-75 days, the alpha-calcium sulfate hemihydrate is matched with the osteogenesis rate of different parts of a human body, and the alpha-calcium sulfate hemihydrate can be used in the field of medical implanted bone repair.

Description

technical field

[0001] The invention relates to a method used in the technical field of biomedical materials for bone tissue repair. Specifically, the patent of the invention provides a method for preparing high-purity surgical grade α-calcium sulfate hemihydrate with adjustable crystal size. Background technique

[0002] Materials for repairing bone defects can generally be divided into three types: autologous bone, allogeneic bone, and synthetic bone according to the source of the material. Autologous bone has osteoconductive, osteoinductive, and osteogenic properties and is considered the gold standard material for repairing bone defects, but the source of autologous bone is limited and requires a second operation. Although allograft bone has osteoconductivity, it also has many disadvantages, such as allograft bone has antigenicity and may transmit pathogens, limited sources and some social and ethical reasons. Therefore, it has driven the rapid development of research o...

Examples

Embodiment 1

[0031] A kind of high-purity crystal size is the preparation method of α-calcium sulfate hemihydrate of 40-50m, and the steps are as follows:

[0032] Weighed 0.1 g of citric acid and 0.4 g of aluminum sulfate and placed them in a 250 mL beaker, and added 150 mL of deionized water into the beaker, and ultrasonically dissolved them for 2 minutes to obtain a reaction solvent solution. Weigh 50g of calcium sulfate dihydrate and place it in a beaker, and stir it mechanically to make it evenly mixed.

[0033] The beaker was placed in an autoclave, the reaction temperature was 120° C., the reaction pressure was 0.11 MPa, and the reaction time was 2 hours.

[0034] After the reaction, the crude product was taken out, filtered and washed 5 times with 80% alcohol to obtain the product.

[0035] The product was dried in a vacuum oven at 60°C for 3 hours, and then vacuum-packed after drying.

[0036] Performance Characterization:

[0037] The α-calcium sulfate hemihydrate prepared in ...

Embodiment 2

[0044] In the present embodiment, a kind of high-purity crystal size is the preparation method of α-calcium sulfate hemihydrate of 30-40m, and the steps are as follows:

[0045] Weigh 0.1 g of citric acid and 0.3 g of aluminum sulfate and place them in a 250 mL beaker, and add 100 mL of deionized water into the beaker, and ultrasonically dissolve for 3 minutes to obtain a reaction solvent. Weigh 50g of calcium sulfate dihydrate and place it in a beaker, and stir it mechanically to make it evenly mixed.

[0046] The beaker was placed in an autoclave, the reaction temperature was 125° C., the reaction pressure was 0.14 MPa, and the reaction time was 1.5 h.

[0047] After the reaction, the crude product was taken out, filtered and washed 5 times with 85% alcohol to obtain the product.

[0048] The product was dried in a vacuum oven at 60°C for 2.5 hours, and then vacuum-packed after drying.

[0049] Performance Characterization:

[0050] The α-calcium sulfate hemihydrate prepa...

Embodiment 3

[0055] In the present embodiment, a kind of high-purity crystal size is the preparation method of α-calcium sulfate hemihydrate of 20-30m, and the steps are as follows:

[0056] Weigh 0.05g of citric acid and 0.035g of aluminum sulfate respectively and place them in a 250mL beaker, and add 50mL of deionized water into the beaker, and ultrasonically dissolve for 4min to obtain a reaction solvent. Weigh 50g of calcium sulfate dihydrate and place it in a beaker, and stir it mechanically to make it evenly mixed.

[0057] The beaker was placed in an autoclave, the reaction temperature was 130° C., the reaction pressure was 0.18 MPa, and the reaction time was 1.5 h.

[0058] After the reaction, the crude product was taken out, filtered and washed 5 times with 90% alcohol to obtain the product.

[0059] The product was dried in a vacuum oven at 60°C for 2 hours, and then vacuum-packed after drying.

[0060] Performance Characterization:

[0061] The α-calcium sulfate hemihydrate p...

technical field

[0001] The invention relates to a method used in the technical field of biomedical materials for bone tissue repair. Specifically, the patent of the invention provides a method for preparing high-purity surgical grade α-calcium sulfate hemihydrate with adjustable crystal size. Background technique

[0002] Materials for repairing bone defects can generally be divided into three types: autologous bone, allogeneic bone, and synthetic bone according to the source of the material. Autologous bone has osteoconductive, osteoinductive, and osteogenic properties and is considered the gold standard material for repairing bone defects, but the source of autologous bone is limited and requires a second operation. Although allograft bone has osteoconductivity, it also has many disadvantages, such as allograft bone has antigenicity and may transmit pathogens, limited sources and some social and ethical reasons. Therefore, it has driven the rapid development of research o...

Examples

Embodiment 1

[0031] A kind of high-purity crystal size is the preparation method of α-calcium sulfate hemihydrate of 40-50m, and the steps are as follows:

[0032] Weighed 0.1 g of citric acid and 0.4 g of aluminum sulfate and placed them in a 250 mL beaker, and added 150 mL of deionized water into the beaker, and ultrasonically dissolved them for 2 minutes to obtain a reaction solvent solution. Weigh 50g of calcium sulfate dihydrate and place it in a beaker, and stir it mechanically to make it evenly mixed.

[0033] The beaker was placed in an autoclave, the reaction temperature was 120° C., the reaction pressure was 0.11 MPa, and the reaction time was 2 hours.

[0034] After the reaction, the crude product was taken out, filtered and washed 5 times with 80% alcohol to obtain the product.

[0035] The product was dried in a vacuum oven at 60°C for 3 hours, and then vacuum-packed after drying.

[0036] Performance Characterization:

[0037] The α-calcium sulfate hemihydrate prepared in ...

Embodiment 2

[0044] In the present embodiment, a kind of high-purity crystal size is the preparation method of α-calcium sulfate hemihydrate of 30-40m, and the steps are as follows:

[0045] Weigh 0.1 g of citric acid and 0.3 g of aluminum sulfate and place them in a 250 mL beaker, and add 100 mL of deionized water into the beaker, and ultrasonically dissolve for 3 minutes to obtain a reaction solvent. Weigh 50g of calcium sulfate dihydrate and place it in a beaker, and stir it mechanically to make it evenly mixed.

[0046] The beaker was placed in an autoclave, the reaction temperature was 125° C., the reaction pressure was 0.14 MPa, and the reaction time was 1.5 h.

[0047] After the reaction, the crude product was taken out, filtered and washed 5 times with 85% alcohol to obtain the product.

[0048] The product was dried in a vacuum oven at 60°C for 2.5 hours, and then vacuum-packed after drying.

[0049] Performance Characterization:

[0050] The α-calcium sulfate hemihydrate prepa...

Embodiment 3

[0055] In the present embodiment, a kind of high-purity crystal size is the preparation method of α-calcium sulfate hemihydrate of 20-30m, and the steps are as follows:

[0056] Weigh 0.05g of citric acid and 0.035g of aluminum sulfate respectively and place them in a 250mL beaker, and add 50mL of deionized water into the beaker, and ultrasonically dissolve for 4min to obtain a reaction solvent. Weigh 50g of calcium sulfate dihydrate and place it in a beaker, and stir it mechanically to make it evenly mixed.

[0057] The beaker was placed in an autoclave, the reaction temperature was 130° C., the reaction pressure was 0.18 MPa, and the reaction time was 1.5 h.

[0058] After the reaction, the crude product was taken out, filtered and washed 5 times with 90% alcohol to obtain the product.

[0059] The product was dried in a vacuum oven at 60°C for 2 hours, and then vacuum-packed after drying.

[0060] Performance Characterization:

[0061] The α-calcium sulfate hemihydrate p...

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