Preparation method of a biomaterial, dihydroxyl calcium phosphate

Abstract

The present application relates to a kind of biological medical materials dicalcium phosphate dihydrate preparation method, technical implementation includes the following steps: preparation of precipitating solvent, preparation of certain concentration CaCl2 And 100mL of Na2CO3 Solution;Reaction bottom solution preparation, according to the volume ratio 1:1, take certain amount of deionized water and anhydrous ethanol, add to the three neck flask placed in oil bath pot, and a certain amount of H3PO4 is added to the bottle, finally, the prepared CaCl2 Solution is added, and is stirred uniformly by magnetic force;Dicalcium phosphate dihydrate preparation process, the prepared Na2CO3 Solution is added to the three neck flask at a certain rate, and stirring rate, reaction temperature and reaction time are controlled;After reaction, washing, suction filtration, drying dicalcium phosphate dihydrate is obtained.The characteristics of the method are: using deionized water / anhydrous ethanol mixed system to prepare dicalcium phosphate dihydrate.Process operation is simple, product crystallinity is good, and purity is high.The obtained dicalcium phosphate dihydrate product has flaky morphology, and can be used as calcium phosphate cement powder, bone repair bracket, toothpaste additive.

Description

Technical Field

[0001] This invention relates to orthopedic and dental materials for use in the biomedical field, and more specifically to a method for preparing a biomedical material, calcium hydrogen phosphate dihydrate. Background Technology

[0002] Irregular bone loss and bone injury grafting are significant challenges in modern surgery. Currently, clinical medicine primarily relies on bone grafts and bone repair materials to treat patients, hoping to achieve bone repair and even reconstruction.

[0003] Bone grafts are classified into autologous bone and allogeneic bone based on their source. Autologous bone has a strong ability to induce osteogenesis and a high fusion rate, but it requires an additional incision on the patient, increasing trauma, and is not suitable for large-scale bone grafting. Allogeneic bone has a wide availability and unlimited usage, but due to individual differences, rejection reactions often occur, increasing the difficulty and cost of treatment. Therefore, bone repair materials have become the key to solving this problem.

[0004] Bone cement is a common name for bone cementing agents, mainly composed of powders, liquids, and additives. It is a type of bone repair material. Calcium phosphate bone cement is one such bone cement material, initially developed by Brown and Chow in 1985. Due to its excellent biocompatibility, osteoinductive properties, and self-curing ability, and because it is similar to the mineral composition of natural bone, it can be absorbed and promotes the inward growth and remodeling of natural bone, making it one of the most promising bone repair materials currently under research.

[0005] Brushite (CaHPO4·2H2O), an active component of calcium phosphate bone cement, is also a precursor of hydroxyapatite. It is a colorless and odorless crystalline powder with excellent biocompatibility and bioactivity, making it a biomedical material. Clinical studies have shown that after transplantation, dicalcium phosphate dihydrate composites readily undergo hydration, releasing calcium and phosphorus ions that can be absorbed by the body and enter the systemic circulatory system, gradually forming new bone tissue. Due to these superior properties, dicalcium phosphate dihydrate has attracted increasing attention from scholars in various fields.

[0006] Given the significant future market demand for calcium phosphate dihydrate, and the fact that current preparation methods generally suffer from high production costs, low product purity, and environmental pollution due to incomplete reactions, this invention provides a method for preparing calcium phosphate dihydrate, a biomedical material, that is low-cost, simple in process, and produces high-quality products. Summary of the Invention

[0007] To overcome the shortcomings of existing technologies and optimize production methods, this invention provides a method for preparing the biomedical material calcium phosphate dihydrate. The product obtained by this method exhibits excellent crystallinity and a flake-like morphology, and causes minimal environmental pollution.

[0008] To achieve the above objectives, the technical solution adopted by the present invention consists of the following steps:

[0009] A method for preparing a biomedical material, calcium hydrogen phosphate dihydrate, specifically includes the following steps:

[0010] (1) Preparation of precipitation solvent. Prepare 100 mL each of CaCl2 and Na2CO3 solutions of a certain concentration for later use.

[0011] (2) Preparation of the reaction base solution. Take a certain amount of deionized water and anhydrous ethanol in a volume ratio of 1:1 and add them to a three-necked flask placed in an oil bath. Then add a certain amount of H3PO4 to the flask and finally add the CaCl2 solution of a certain concentration prepared in step (1). Stir magnetically to mix evenly.

[0012] (3) Preparation process of calcium hydrogen phosphate dihydrate. The Na2CO3 solution prepared in step (1) is added dropwise at a certain rate to the three-necked flask containing the prepared deionized water / anhydrous ethanol / H3PO4 / CaCl2 reaction base solution in step (2) through a dropping funnel. The preparation process is carried out under certain stirring rate, reaction temperature and reaction time.

[0013] (4) After the preparation process in step (3) is completed, wash, filter and dry to obtain the product of dicalcium phosphate dihydrate.

[0014] Preferably, in step (1), the concentration of CaCl2 is 0.15 mol / L to 0.75 mol / L, and the concentration of Na2CO3 is 0.05 mol / L to 0.25 mol / L.

[0015] Preferably, in step (2), 100 mL each of the deionized water, anhydrous ethanol (AR), and CaCl2 solution are taken, 1-2 mL of H3PO4 (AR) is added, the stirring temperature is 25°C, the stirring speed is 100-300 rpm, and the stirring time is 30 min.

[0016] Preferably, in step (3), the dropping rate of the Na2CO3 solution is 6-10 mL / min, the stirring speed is 100-300 rpm, the reaction temperature is 50-70℃, and the reaction time is 3-5 h.

[0017] Preferably, in step (4), after the preparation process is completed, the product is washed three times with deionized water, filtered by a vacuum pump, and dried at a temperature of 60-80°C for 8-10 hours.

[0018] Compared with existing methods, the present invention has the following advantages:

[0019] 1. This invention uses an ethanol / water mixed system to prepare calcium hydrogen phosphate dihydrate. The reaction can proceed spontaneously, the preparation process is simple, the conditions are controllable and easy to operate, and the product has excellent crystallinity, which fully meets market demand.

[0020] 2. The raw materials for this invention are readily available, the conditions are controllable, and it does not require high temperature or high pressure, resulting in low production costs and fewer preparation steps. This greatly saves on cost and manpower. Attached Figure Description

[0021] Figure 1 XRD pattern of calcium hydrogen phosphate dihydrate obtained in Example 1

[0022] Figure 2 Field emission scanning electron microscope image of calcium hydrogen phosphate dihydrate obtained in Example 1.

[0023] Figure 3 Field emission scanning electron microscope image of calcium hydrogen phosphate dihydrate obtained in Example 2.

[0024] Figure 4 Field emission scanning electron microscope image of calcium hydrogen phosphate dihydrate obtained in Example 3. Detailed Implementation

[0025] The technical solution of the present invention will now be described in detail through specific embodiments.

[0026] Example 1

[0027] A method for preparing a biomedical material, calcium phosphate dihydrate, comprising the following production steps:

[0028] (1) Preparation of precipitation solvent. Prepare 100 mL each of 0.15 mol / L CaCl2 solution and 0.05 mol / L Na2CO3 solution for later use;

[0029] (2) Preparation of reaction base solution. Take 100 mL of deionized water and anhydrous ethanol in a volume ratio of 1:1 and add them to a three-necked flask placed in an oil bath. Then add 1 mL of H3PO4 to the flask. Finally, add all of the 0.15 mol / L CaCl2 solution prepared in (1) and stir magnetically at 25°C for 30 min to mix evenly.

[0030] (3) Preparation process of calcium hydrogen phosphate dihydrate. The Na2CO3 solution prepared in step (1) was added dropwise at a rate of 6 mL / min to the three-necked flask containing the prepared deionized water / anhydrous ethanol / H3PO4 / CaCl2 reaction base solution in step (2) through a dropping funnel. The preparation process was carried out at a stirring rate of 100 rpm, a reaction temperature of 50 °C, and a reaction time of 3 h.

[0031] (4) After the preparation process in step (3) is completed, wash with deionized water three times, filter by vacuum pump, and dry at 60°C for 8 hours to obtain the product of dicalcium phosphate dihydrate.

[0032] Example 2

[0033] A method for preparing a biomedical material, calcium phosphate dihydrate, comprising the following production steps:

[0034] (1) Preparation of precipitation solvent. Prepare 100 mL each of 0.45 mol / L CaCl2 solution and 0.15 mol / L Na2CO3 solution for later use;

[0035] (2) Preparation of reaction base solution. Take 100 mL of deionized water and anhydrous ethanol in a volume ratio of 1:1 and add them to a three-necked flask placed in an oil bath. Then add 1.5 mL of H3PO4 to the flask. Finally, add all of the 0.45 mol / L CaCl2 solution prepared in (1) and stir magnetically at 25 °C for 30 min to mix evenly.

[0036] (3) Preparation process of calcium hydrogen phosphate dihydrate. The Na2CO3 solution prepared in step (1) was added dropwise at a rate of 6 mL / min to the three-necked flask containing the prepared deionized water / anhydrous ethanol / H3PO4 / CaCl2 reaction base solution in step (2) through a dropping funnel. The preparation process was carried out at a stirring rate of 100 rpm, a reaction temperature of 60 °C, and a reaction time of 4 h.

[0037] (4) After the preparation process in step (3) is completed, wash with deionized water three times, filter by vacuum pump, and dry at 70°C for 9 hours to obtain the product of dicalcium phosphate dihydrate.

[0038] Example 3

[0039] A method for preparing a biomedical material, calcium phosphate dihydrate, comprising the following production steps:

[0040] (1) Preparation of precipitation solvent. Prepare 100 mL each of 0.75 mol / L CaCl2 solution and 0.25 mol / L Na2CO3 solution for later use;

[0041] (2) Preparation of reaction base solution. Take 100 mL of deionized water and anhydrous ethanol in a volume ratio of 1:1 and add them to a three-necked flask placed in an oil bath. Then add 2 mL of H3PO4 to the flask. Finally, add all of the 0.75 mol / L CaCl2 solution prepared in (1) and stir magnetically at 25°C for 30 min to mix evenly.

[0042] (3) Preparation process of calcium hydrogen phosphate dihydrate. The Na2CO3 solution prepared in step (1) was added dropwise at a rate of 6 mL / min to the three-necked flask containing the prepared deionized water / anhydrous ethanol / H3PO4 / CaCl2 reaction base solution in step (2) through a dropping funnel. The preparation process was carried out at a stirring rate of 100 rpm, a reaction temperature of 70 °C, and a reaction time of 5 h.

[0043] (4) After the preparation process in step (3) is completed, wash with deionized water three times, filter by vacuum pump, and dry at 80°C for 10 hours to obtain the product of dicalcium phosphate dihydrate.

Claims

1. A method for preparing sheet-like calcium hydrogen phosphate dihydrate, a biomedical material, characterized in that, Includes the following steps: (1) Preparation of precipitation solvent: Prepare 100 mL each of CaCl2 and Na2CO3 solutions of a certain concentration for later use. (2) Preparation of reaction base liquid: Take a certain amount of deionized water and anhydrous ethanol at a volume ratio of 1:1 and add them to a three-necked flask placed in an oil bath. Then add a certain amount of H3PO4 to the flask and finally add the CaCl2 solution of a certain concentration prepared in step (1). Stir magnetically to mix evenly. (3) Preparation of flake-shaped calcium hydrogen phosphate dihydrate: The Na2CO3 solution prepared in step (1) is added dropwise through a dropping funnel at a rate of 6-10 mL / min to the three-necked flask containing the deionized water / anhydrous ethanol / H3PO4 / CaCl2 reaction base solution prepared in step (2). The reaction is carried out at a stirring speed of 100-300 rpm and a reaction temperature of 50-70℃ for 3-5 h. (4) After the preparation process in step (3) is completed, wash with deionized water three times, filter by vacuum pump, and dry in an oven at 60-80℃ for 8-10 hours to obtain flaky dicalcium phosphate dihydrate product.

2. The method for preparing sheet-like calcium hydrogen phosphate dihydrate, a biomedical material, according to claim 1, is characterized in that, In step (1), the concentration of the CaCl2 solution is 0.15 mol / L to 0.75 mol / L, and the concentration of the Na2CO3 solution is 0.05 mol / L to 0.25 mol / L.

3. The method for preparing sheet-like calcium hydrogen phosphate dihydrate, a biomedical material, according to claim 1, is characterized in that... In step (2), 100 mL each of the deionized water, AR-grade anhydrous ethanol, and CaCl2 solution are taken, and 1-2 mL of AR-grade H3PO4 is added. The stirring temperature is 25°C, the stirring speed is 100-300 rpm, and the stirring time is 30 min.

4. The method for preparing sheet-like calcium hydrogen phosphate dihydrate, a biomedical material, according to claim 1, is characterized in that, In step (4), the obtained calcium hydrogen phosphate dihydrate is in the form of flakes, with good crystallinity, uniform size, length of 10-70 μm and thickness of 50-100 nm. It can be used in the biomedical field and has good biocompatibility and degradability.

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