Preparation method of waterborne polyurethane (WPU)/collagen/hydroxyapatite (HAP) composite material

A water-based polyurethane, hydroxyapatite technology, applied in the fields of medical science, prosthesis, tissue regeneration, etc., can solve the problems of difficulty in balancing mechanical properties, biological functions and biodegradation properties, lack of osteoinductive activity, and poor plasticity. , to achieve the effects of controllable mechanical processability, good biocompatibility and low cost

Active Publication Date: 2019-09-17
QILU UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, in most cases, HAP bioceramics prepared by high temperature have disadvantages such as poor plasticity, brittle texture, and lack of osteoinductive activity, and it is difficult to properly balance mechanical properties, biological functions, and biodegradable properties.

Method used

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  • Preparation method of waterborne polyurethane (WPU)/collagen/hydroxyapatite (HAP) composite material
  • Preparation method of waterborne polyurethane (WPU)/collagen/hydroxyapatite (HAP) composite material
  • Preparation method of waterborne polyurethane (WPU)/collagen/hydroxyapatite (HAP) composite material

Examples

Experimental program
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Embodiment 1

[0048] Example 1, a method for preparing a water-based polyurethane / collagen / hydroxyapatite composite material, the material is prepared using a glass three-necked flask, equipped with vacuum dehydration, heating and cooling, condensation reflux, constant pressure dripping device, including the following steps :

[0049] (1) Weigh 50 g of polyethylene adipate diol (molecular weight: 2000), vacuum dehydrate at 110°C for 1~2 h, cool down to 60°C, add 45 g of diphenylmethane diisocyanate to react 1 h, be warming up to 82 DEG C, be incubated 1 h and obtain prepolymer;

[0050](2) In step (1), the temperature of the prepolymer was lowered to 60°C, and 5 g of dimethylolpropionic acid was added for chain extension, and reacted for 1 h, and then 8 g of diethylene glycol was added to the system for Chain extension, after reacting for 30 minutes, raise the temperature to 82°C and keep it warm for 2-3 hours until -NCO is close to the theoretical value (detected by di-n-butylamine method...

Embodiment 2

[0055] Embodiment 2, a kind of preparation method of aqueous polyurethane / collagen protein / hydroxyapatite composite material, comprises the following steps:

[0056] (1) Weigh 50 g of polytrimethylene adipate diol (molecular weight 2000), vacuum dehydrate at 105°C for 1~2 h, cool down to 60°C, add 30 g of toluene diisocyanate, react for 1 h, and heat up to 82 ° C, incubated for 1 h to obtain the prepolymer;

[0057] (2) Cool the prepolymer to 60°C in step (1), add 5 g of dimethylolpropionic acid for chain extension, react for 1 h, add 3 g of propylene glycol to the system for chain extension, and react for 30 min, Heat up to 80°C, keep warm for 2-3 hours;

[0058] (3) Cool the product in step (2) to 50°C, add 3.5 g of triethylamine for neutralization, and add an appropriate amount of acetone to adjust the viscosity. After being cooled to room temperature, add 5 DEG C of deionized water 1100r / min and stir for 5 min to obtain an aqueous polyurethane prepolymer emulsion;

[00...

Embodiment 3

[0062] Embodiment 3, a kind of preparation method of aqueous polyurethane / collagen protein / hydroxyapatite composite material, comprises the following steps:

[0063] (1) Weigh 40 g isophorone diisocyanate, 50 g polybutylene adipate diol (molecular weight 2000) after vacuum dehydration, 1~2 drops of dibutyltin dilaurate catalyst, at 65°C Reaction 1 h, be warming up to 80 ℃, insulation 1~2 h obtains prepolymer;

[0064] (2) Add 6 g of dihydroxybutyric acid to the prepolymer in step (1) for chain extension, react at 60°C for 1 h, add 7 g of diethylene glycol to the system for chain extension, and keep warm at 60°C for 1 hour h, be warming up to 80 DEG C, react 2~3 h;

[0065] (3) Cool the product in step (2) to 50°C, add 4 g of triethylamine for neutralization, and adjust the viscosity with an appropriate amount of acetone. After being cooled to room temperature, add 5 DEG C of deionized water 1200r / min and stir for 5 min to obtain an aqueous polyurethane prepolymer emulsion; ...

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Abstract

The invention discloses a preparation method of a waterborne polyurethane (WPU)/collagen/hydroxyapatite (HAP) composite material. The composite material is prepared from the following components in parts by weight: diisocyanate, polyester polyol, a chain extender, a waterborne chain extender, a neutralizer, a hydrolyzed collagen solution, gamma-glycidoxypropyltrimethoxysilane (KH560), calcium chloride and sodium hydrogen phosphate. According to the preparation method, an emulsion polymerization reaction is performed on a polyester-type WPU prepolymer and a biochemical-level gelatin hydrolysate (GH), and external crosslink modification is further performed through KH560 to improve the hydrophobicity and adhesive film toughness of the material, thus preparing a WPU and GH graft copolymerization composite emulsion (WPU-g-GH). The invention aims to prepare the nano HAP composite material with good mechanical property, structural stability, biocompatibility and degradability, which is expected to be a potential bone scaffold repair material.

Description

technical field [0001] The invention relates to a preparation method of a water-based polyurethane / collagen / hydroxyapatite composite material, belonging to the field of biomedical polymer materials. Background technique [0002] Bone defects are usually caused by congenital diseases, trauma, infection, tumors. The use of autografts and allografts to replace and repair bone defects has been limited due to supply shortages, additional complications, and immune rejection. [0003] Therefore, designing and manufacturing artificial bone repair or substitutes with good mechanical properties, biocompatibility, biodegradability and porous structure by simulating the formation mechanism of natural tissues has become an important research direction in recent years. Bone is essentially a biological composite of inorganic minerals and collagen. Hydroxyapatite (HAP, Ca 10 (PO 4 ) 6 (OH) 2 ) nanocrystals, as an important inorganic mineral in bone tissue, have been widely studied and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G18/83C08G18/66C08G18/64C08G18/48C08G18/34C08G18/32C08G18/10C08K3/32A61L27/46A61L27/58
CPCA61L27/46A61L27/58A61L2300/412A61L2430/02C08G18/10C08G18/4238C08G18/6446C08G18/837C08K3/32C08K2003/325C08G18/348C08G18/3206C08G18/64C08L75/06
Inventor 杨茂张敏李彦春祝德义鹿文慧
Owner QILU UNIV OF TECH
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