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Catalyst for preparing p-dioxanone and method for preparing p-dioxanone

A technology for dioxanone and catalysts, applied in metal/metal oxide/metal hydroxide catalysts, chemical instruments and methods, chemical elements of heterogeneous catalysts, etc., can solve the problem of reducing the number of strong acid centers and desorption. Increase in strength, short catalyst life and other problems, achieve the effect of increasing desorption strength, improving selectivity, and solving low yield

Pending Publication Date: 2021-03-12
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The first object of the present invention is to provide a catalyst for preparing p-dioxanone, which follows the purpose of green chemistry, and solves the problems of low yield, easy polymerization, difficult purification and low production rate in the traditional preparation of p-dioxanone Catalyst life is short and other problems, while the present invention prepares catalyst raw materials with few types, simple catalyst reaction process, simple product purification method and high yield, thereby greatly reducing the cost of preparing p-dioxanone, which has industrial value
The main active components of the catalyst are copper oxide and silicon oxide, which solves the problems of low yield, easy polymerization, difficult purification and short catalyst life in the traditional preparation process of dioxanone. The process is simple, and at the same time, the basic position of sodium oxide is used to increase the desorption strength of the weak acid center of the catalyst, thereby reducing the number of strong acid centers, effectively inhibiting the dehydration of diethylene glycol to produce 1.4-dioxane, and improving the target The selectivity of the product to dioxanone, and the control of the reaction temperature to avoid carbon deposition on the catalyst

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Embodiment 1: A kind of catalyst for preparing p-dioxanone and the method for preparing p-dioxanone

[0030] (1) Preparation method of copper-silicon catalyst:

[0031] S1. First weigh 25.2g of sodium bicarbonate and dissolve it in 478.8g of water, stir at 60°C and 100r / min, weigh 62.5g of tetraethyl orthosilicate and drop it into the sodium bicarbonate solution through a constant pressure dropping funnel;

[0032] S2. Weigh again 36.2g of copper nitrate trihydrate dissolved in 253.2g of water and continue to add dropwise. After the dropwise addition is complete, the pH is 7.5. Continue to react for 1h, age at 20°C for 2h, wash twice and then filter with suction;

[0033] S3. The precipitate after suction filtration was dried at 90°C for 8 hours, and then calcined at 400°C for 4 hours; characterized by ICP, the content of copper oxide was 46.2%, sodium oxide was 1%, and the rest was silicon dioxide. Characterized by BET, the specific surface area of ​​the catalyst is 2...

Embodiment 2

[0038] Embodiment 2: A kind of catalyst for preparing p-dioxanone and the method for preparing p-dioxanone

[0039] (1) Preparation method of copper-silicon catalyst:

[0040] S1. First weigh 25.2g of sodium bicarbonate and dissolve it in 478.8g of water, stir at 90°C and 400r / min, weigh 62.5g of tetraethyl orthosilicate and drop it into the sodium bicarbonate solution through a constant pressure dropping funnel;

[0041] S2. Weigh again 36.2g of copper nitrate trihydrate dissolved in 253.2g of water and continue to add dropwise. After the dropwise addition is complete, the pH is 7.5, continue to react for 1h, age at 20°C for 12h, wash 5 times and then filter;

[0042] S3. The filtered precipitate was dried at 90°C for 24 hours and calcined at 400°C for 4 hours; characterized by ICP, the content of copper oxide was 46.6%, sodium oxide was 0.6%, and the rest was silicon dioxide. Characterized by BET, the specific surface area of ​​the catalyst is 40m 2 / g, pore size 10nm.

...

Embodiment 3

[0047] Embodiment 3: A kind of catalyst for preparing p-dioxanone and the method for preparing p-dioxanone

[0048] (1) Preparation method of copper-silicon catalyst:

[0049] S1. First weigh 25.2g of sodium bicarbonate and dissolve it in 226.8g of water, stir at 80°C and 300r / min, weigh 62.5g of tetraethyl orthosilicate and drop it into the sodium bicarbonate solution through a constant pressure dropping funnel;

[0050] S2. Weigh again 36.2g of copper nitrate trihydrate dissolved in 253.2g of water and continue to add dropwise. After the dropwise addition is complete, the pH is 7.5. Continue to react for 1h, age at 20°C for 12h, wash 8 times and then filter;

[0051] S3. The filtered precipitate was dried at 90°C for 8 hours and calcined at 400°C for 4 hours. According to ICP, the content of copper oxide was 46.9%, sodium oxide was 0.1%, and the rest was silicon dioxide. Characterized by BET, the specific surface area of ​​the catalyst is 42m 2 / g, pore size 11nm.

[0052...

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Abstract

The invention belongs to the technical field of catalyst dehydrogenation, and particularly relates to a catalyst for preparing p-dioxanone and a method for preparing p-dioxanone. The technical key point is as follows: the copper-silicon catalyst comprises the following components in percentage by weight: 46.2%-46.9% of copper oxide, 0.1%-1% of sodium oxide and the balance of silicon dioxide. The preparation process follows the purpose of green chemistry, solves the problems of low yield, easy polymerization, difficult purification, short catalyst life and the like in the traditional p-dioxanone preparation process, and has the advantages of few catalyst raw material types, simple catalyst reaction process, simple product purification method, high yield and low cost. The preparation cost ofp-dioxanone is greatly reduced, and the industrial value is achieved.

Description

technical field [0001] The invention belongs to the technical field of catalyst dehydrogenation, and in particular relates to a catalyst for preparing p-dioxanone and a method for preparing p-dioxanone. Background technique [0002] Polydioxanone has excellent biocompatibility, bioabsorbability and biodegradability, it is an ideal surgical suture material, and can also be used to manufacture bone plates and tissue repair materials, such as screws, hooks , sheet and forceps and other surgical instruments, has a wide range of application prospects. [0003] The preparation of polydioxanone with excellent properties requires the synthesis of high-purity monomeric p-dioxanone. The synthesis of dioxanone began in the 1930s, reported by Raymond W, John Ban and Howard R et al. The principle of its synthesis is based on the catalytic dehydrogenation of diethylene glycol. The specific synthesis process is as follows: at a temperature of 240-360°C, the steam of diethylene glycol pas...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/78C07D319/12B01J35/10
CPCB01J23/002B01J23/78C07D319/12B01J2523/00B01J35/613B01J35/647B01J2523/12B01J2523/17B01J2523/41
Inventor 钱俊峰何天赐孙中华何明阳陈群吴中
Owner CHANGZHOU UNIV