Preparation method of polypara dioxo cyclohexanone capable of raising molecular weight and conversion rate simultaneously

A technology for poly-p-dioxanone and p-dioxanone is applied in the field of preparation of poly-p-dioxanone, which can solve the problem of only 62% of the monomer conversion rate, and achieves the improvement of the monomer conversion rate. , good economic benefits, easy to control effect

Active Publication Date: 2006-05-17
成都普利铭医用材料科技有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But at 100°C, when the M / C is 2000 / 1, the viscosity can only reach 0.95dL / g after 14 hours of reaction, and the monomer conversion rate is only 62%.
In 2000, Japan's Nishida, (Macromolecules 2000, 33, 6982-6986.) and others adopted stannous octoate catalyst to realize the ring-opening polymerization of dioxanone under the condition that there is no co-initiator, although at 100 Under the condition of ℃, when the M / C is 4900 / 1, after 20 hours of reaction, the molecular weight of the polymer reaches 142,000, but the monomer conversion rate is only 79.4%.
In 2000, Raquez (Macromol. Rapid Commun. 2000, 21, 1063-1071.) and others also realized the ring-opening polymerization of dioxanone by using aluminum triisopropoxide as a catalyst. The intrinsic viscosity [η] of cyclohexanone increases with the ratio M / I of monomer and aluminum triisopropoxide, which has good controllability, but the synthesized polydioxanone product is the highest The intrinsic viscosity is only 0.77dL / g, and the monomer conversion rate is only 70%.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] This example uses AlEt 3 -Nb(AcAc) 3 -H 2 O catalyst for the preparation of polydioxanone. All operations are carried out under the protection of anhydrous, oxygen-free and high-purity nitrogen.

[0019] 1. Preparation of catalyst: add neodymium acetylacetonate (Nb(AcAc) 3 ) and anhydrous toluene, and then inject triethylaluminum (AlEt 3 ) and aged at 60°C for 2 hours under the protection of nitrogen, and slowly added a mixed solution (H 2 O / DXO=1 / 9), after the reaction stopped, it was lowered to room temperature for later use. Et 3 with Nb(AcAc) 3 The molar ratio is 8:1, H 2 O and AlEt 3 The molar ratio is 0.5:1.

[0020] 2. Polymerization: Add 3.6 grams of p-dioxanone with a purity of more than 99.5% and a water content of 120 ppm into a polymerization bottle that has been baked at high temperature and repeatedly evacuated and ventilated with nitrogen, and then add the prepared Et 3 -Nb(AcAc) 3 -H 2 15.7 microliters of O catalyst was sealed and then stir...

Embodiment 2

[0024] This example uses AlEt 3 -H 3 PO 4 -H 2 O catalyst for the preparation of polydioxanone. All operations are carried out under the protection of anhydrous, oxygen-free and high-purity nitrogen.

[0025] 1. The preparation method of the catalyst is completely the same as in Example 1, so it is omitted. The difference is the proportioning ratio of each component of the catalyst of this embodiment: AlEt 3 with H 3 PO 4 The molar ratio is 8:1, H 2 O and AlEt 3 The molar ratio is 0.5:1.

[0026] 2. Polymerization: Add 3.6 grams of p-dioxanone with a purity of more than 99.5% and a water content of 73 ppm into a polymerization bottle that has been baked at high temperature and repeatedly evacuated and vented with nitrogen, and then add the prepared Et 3 -H 3 PO 4 -H 2 15.7 microliters of O catalyst was sealed and then stirred and polymerized in a constant temperature oil bath at 100°C for 3 hours to obtain the reaction product. The molar ratio of dioxanone and c...

Embodiment 3

[0030] This example uses AlEt 3 -H 2 O catalyst for the preparation of polydioxanone. All operations are carried out under the protection of anhydrous, oxygen-free and high-purity nitrogen.

[0031] 1. Preparation of the catalyst: Add triethylaluminum (AlEt 3 ), and slowly dropwise added a mixed solution of water and 1,4 dioxane (DXO) under stirring (H 2 O / DXO=1 / 9), after the generated gas stops, cool down to room temperature for later use. h 2 O and AlEt 3 The molar ratio is 0.1:1.

[0032] 2. Polymerization: Add 3.6 grams of p-dioxanone with a purity of more than 99.5% and a water content of 85 ppm in a polymerization bottle that has been baked at high temperature and repeatedly evacuated and vented with nitrogen, and then add the prepared Et 3 -H 2 31.4 microliters of O catalyst was sealed and stirred and polymerized in a constant temperature oil bath at 60°C for 6 hours to obtain the reaction product. The molar ratio of dioxanone to catalyst is 5000:1.

[0033] ...

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Abstract

The preparation method of the polydioxanone disclosed by the invention can increase the molecular weight and conversion rate at the same time. The method is to mix the p-dioxanone and the catalyst in a molar ratio of 800 to 10000:1 in the Under the protection of anhydrous, oxygen-free and inert gas, heat to 40-160°C to polymerize to obtain the reaction product; purify and dry the obtained reaction product to obtain the purified product, which is characterized in that the catalyst is an alkylaluminum intercombination catalytic system or Isopropanol rare earth salt; polymerization time 3-10 hours. The process method of the invention is mature, simple, easy to control, and has a short production cycle. While obtaining polydioxanone with a molecular weight of 70,000-810,000, the monomer conversion rate can reach more than 84.5%.

Description

1. Technical field [0001] The invention belongs to the technical field of polydioxanone preparation, and in particular relates to a preparation method of polydioxanone capable of simultaneously increasing molecular weight and conversion rate. 2. Background technology [0002] As a new material, polydioxanone was first developed by Ethicon in the United States in the late 1970s. Due to the unique ether bond contained in the molecular chain of polydioxanone, the flexibility of the molecular chain is good, so that it has been widely used. Among them, high molecular weight polydioxanone can be widely used in surgical sutures, screws, fixed bolts, pins, anchors, hoops, hemostatic forceps, hemostatic plaster, suture clips, pharmaceutical screens, and medical adhesives. Orthopedic fixation materials, tissue repair materials and framework materials for drug sustained release systems. [0003] Although since the 1970s, people have successively adopted stannous octoate (SnOct 2 ), ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/664
Inventor 王玉忠郭跃海杨科珂汪秀丽周茜郑长义陈泽芳
Owner 成都普利铭医用材料科技有限责任公司
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