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Method for preparing hydroxyapatite-natural macromolecular nano compound with one-pot method

A technology of natural polymer and hydroxyapatite is applied in the field of preparing hydroxyapatite-natural polymer nanocomposite by one-pot method, which can solve the problems of simple operation of raw material powder, single product obtaining method, cumbersome and time-consuming, etc. To achieve the effect of simple method, saving water resources and low energy consumption

Inactive Publication Date: 2016-05-25
HUBEI SAILUO BIOLOGICAL MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The Chinese patent "Preparation method of linear nano-hydroxyapatite" (publication number CN102491298B) discloses a method for preparing linear nano-hydroxyapatite, specifically, the first mass concentration of silk fibroin aqueous solution is concentrated to the second After the mass concentration is sealed and cultivated, the obtained silk fibroin nanofiber aqueous solution is mixed with the phosphate source and the calcium source, and the linear nano-hydroxyapatite is obtained after the reaction. The key point of this method is the repeated drying of the silk fibroin aqueous solution. operation, which is quite complex
The Chinese patent "Mineralized Silk Protein Material and Its Preparation Method" (publication number CN1241654C) discloses a mineralized silk protein material and its preparation method, wherein the organic component is degummed silk protein, and the minerals are calcium phosphorus salt crystals. The specific method It is to add calcium ion-containing solution and phosphate ion-containing solution to the water-soluble degummed silk protein solution under stirring, adjust the pH value of the reaction system, keep stirring for a while, then let the system stand still, repeat centrifugation, wash the precipitate, and then put Precipitation is vacuum dried to obtain the product; however, the system has the problems of non-constant temperature, large capacity, pH deviation from the most stable value of hydroxyapatite, and a single method for obtaining the product
In the Chinese patent "Hydroxyapatite / Chitosan Silk Fibroin Nanocomposite Material and Preparation Method", the silk fibroin solid is mixed with calcium hydroxide emulsion to make liquid A, and the chitosan solution and phosphoric acid are mixed to make liquid B , and then add liquid B to liquid A drop by drop, these operations are cumbersome and time-consuming
In the Chinese patent "Silk Fibroin / Nano-Hydroxyapatite Porous Scaffold Material and Its Preparation Method" (Publication No. CN102000362A), the degummed silk fibroin fibers are dissolved in a calcium oxide ternary solution, and phosphate is added dropwise thereto to obtain Silk fibroin / nano hydroxyapatite powder, but after that the powder is mixed with H 2 o 2 Solution and carboxymethyl cellulose are mixed and foamed to obtain a slurry, and the slurry is freeze-dried after injection molding to obtain a silk fibroin / nano-hydroxyapatite composite porous scaffold material, which is quite different from this patent
[0007] Although there are many researches and patents related to hydroxyapatite and its composite materials, there is still no method that puts the raw material powder directly into the reaction system like the present invention, which is easy to operate, easy to automate, clean reagents, and low in cost.

Method used

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  • Method for preparing hydroxyapatite-natural macromolecular nano compound with one-pot method
  • Method for preparing hydroxyapatite-natural macromolecular nano compound with one-pot method
  • Method for preparing hydroxyapatite-natural macromolecular nano compound with one-pot method

Examples

Experimental program
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Effect test

Embodiment 1

[0049] (1) Weigh 5.02 g of soluble silk fibroin, dissolve in 200 mL of deionized water in a constant temperature water bath at 40° C., and dissolve for 3 hours under stirring at a rotation speed of 1300 rpm to obtain a silk fibroin solution.

[0050](2) The silk fibroin solution is placed in a 40°C constant temperature water bath, and under stirring at a rotating speed of 1300rpm, 12.74g of potassium phosphate is added, and after dissolving, 23.61g of calcium nitrate tetrahydrate is added, and Ca / P= 5:3 (the ratio of the amount of substance), the ratio of the mass of the natural polymer to the mass sum of calcium ions and phosphate ions in the two precursor salts is 0.518. After 5 minutes, add 100mL of ammonia water (NH 3 The concentration is 25-28%), and the stirring speed is adjusted to 650rpm, stirring for 3h to make it fully react.

[0051] (3) After the reaction is completed, the stirring is stopped, and the reaction product is aged for 12 hours at a constant temperature ...

Embodiment 2

[0057] (1) Weigh 5.02 g of soluble silk fibroin, dissolve it in 200 mL of deionized water in a constant temperature water bath at 40° C., and dissolve it for 3 hours under stirring at a rotation speed of 1300 rpm to obtain a silk fibroin solution.

[0058] (2) Put the silk fibroin solution in a constant temperature water bath at 40°C, and add 12.74g of potassium phosphate under stirring at a rotating speed of 1300rpm. After dissolving, add 11.10g of anhydrous calcium chloride. At this time, Ca / P =5:3 (ratio of the amount of substance), the ratio of the quality of the natural polymer to the mass sum of calcium ions and phosphate ions in the two precursor salts is 0.518. After 5 minutes, add 100mL ammoniacal liquor (NH 3 The concentration is 25-28%), and the stirring speed is adjusted to 650rpm, stirring for 9h to make it fully react.

[0059] (3) After the reaction is completed, the stirring is stopped, and the reaction product is aged for 15.5 hours at a constant temperature o...

Embodiment 3

[0065] (1) Weigh 1.01 g of soluble silk fibroin, dissolve it in 40 mL of deionized water in a constant temperature water bath at 40° C., and dissolve it for 3 hours under stirring at a rotation speed of 1300 rpm to obtain a silk fibroin solution.

[0066] (2) The silk fibroin solution is placed in a 40°C constant temperature water bath, and under stirring at a rotating speed of 1300rpm, 1.44g of sodium dihydrogen phosphate is added, and after dissolving, 4.723g of calcium nitrate tetrahydrate is added. At this time, Ca / P=5:3 (ratio of the amount of substance), the ratio of the mass of the natural polymer to the mass sum of calcium ions and phosphate ions in the two precursor salts is 0.521. After 5 minutes, add 20mL of ammonia water (NH 3 The concentration is 25-28%), and the stirring speed is adjusted to 650rpm, stirring for 20h to fully react.

[0067] (3) After the reaction is completed, the stirring is stopped, and the reaction product is aged for 14 hours at a constant t...

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Abstract

The invention discloses a method for preparing a hydroxyapatite-natural macromolecular nano compound with a one-pot method. The method disclosed by the invention has the core characteristics that raw material powder is directly added, and mainly comprises the following steps: adding calcium salt and phosphate into a natural macromolecular solution according to the amount of substance ratio of Ca / P of 5 to 3; adjusting the pH of the system to 10 to 12 by using an alkali solution, wherein calcium ions, phosphate ions and hydroxyl ions in the system and natural macromolecules have an in-situ co-precipitation reaction; washing a reaction product to be neutral, and drying to obtain the hydroxyapatite-natural macromolecular nano compound; grinding and sieving to prepare nano composite particle products with different specifications. The method disclosed by the invention is simple and has moderate reaction conditions and small energy consumption; the obtained hydroxyapatite-natural macromolecular nano compound has good granularity, rigidity, microscopic appearance and crystallinity, and can be widely applied to the fields of bone defect repairing tissue engineering materials and medical equipment and the like of dental department, orthopedic surgery and the like.

Description

technical field [0001] The invention belongs to the technical field of bone tissue engineering materials and medical devices, and in particular relates to a method for preparing hydroxyapatite-natural polymer nanocomposites in one pot. Background technique [0002] Due to the huge market demand, bone tissue substitute materials are a hot spot in the research and application of biomedical materials. The repair effect of endogenous bone tissue is good, but the promotion and use of this therapy is limited due to the shortage of alternative materials; while the repair of exogenous bone tissue has obvious immune rejection, and may also introduce potential pathogens and other toxic side effects. It can be seen that it is of great practical significance to study and prepare an efficient and safe artificial bionic bone tissue replacement material. [0003] Natural bone tissue is a uniform and orderly biological complex composed of inorganic minerals (mainly nano-hydroxyapatite) and...

Claims

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Application Information

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IPC IPC(8): A61L27/46A61L27/58
CPCA61L27/46A61L27/58A61L2400/12A61L2430/02A61L2430/12
Inventor 邓红兵詹颖菲
Owner HUBEI SAILUO BIOLOGICAL MATERIAL CO LTD
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