Preparation method of glycolide

A glycolide and glycolate technology, which is applied in chemical instruments and methods, molecular sieve catalysts, organic chemistry, etc., can solve the problems of catalyst recovery and utilization under harsh conditions for glycolide synthesis, and catalysts that cannot be recycled.

Active Publication Date: 2021-05-14
CHINA CATALYST HLDG CO LTD
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Problems solved by technology

[0005] In view of the current development status of my country's coal chemical industry, we should make full use of the advantages of existing ethylene glycol technology and equipment capacity to develop low-cost methyl glycolate derivative products and applications. In recent years, it has been reported that methyl glycolate is used as a raw material to synthesize ethylene glycol lactide, but the synthesis method is still polycondensation-depolymerization method, and the catalyst is still not recyclable, which fails to fundamentally solve the problem of harsh synthesis conditions of glycolide and catalyst recycling

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preparation example Construction

[0035] The invention provides a preparation method of glycolide.

[0036] In a specific embodiment provided by the present invention, in the preparation method of glycolide, the gaseous glycolate is subjected to a cyclization reaction under the conditions catalyzed by a titanium-containing molecular sieve to obtain the product glycolide.

[0037] The reaction formula of glycolate cyclization synthetic glycolide is as follows:

[0038]

[0039] R can be methyl, ethyl, n-propyl, isopropyl, n-butyl.

[0040] In a specific embodiment provided by the present invention, the titanium-containing molecular sieve is a regular structure titanium-containing molecular sieve.

[0041] The titanium-containing molecular sieve with regular structure mentioned in the present invention refers to a titanium-containing molecular sieve with high crystallinity and regular appearance.

[0042] In a specific embodiment provided by the present invention, the titanium-containing molecular sieve is ...

Embodiment 1

[0069] The preparation of embodiment 1 titanium silicon molecular sieve TS-1

[0070] With silica sol (silicon dioxide content is 30wt%) as silicon source, tetrabutyl titanate as titanium source, tetrapropyl ammonium bromide as template, silica sol, tetrabutyl titanate, tetrapropyl ammonium bromide The mass ratio is 91.5:4:4.5, crystallized at 180°C for 30h, filtered, washed, dried and calcined to obtain titanium silicon molecular sieve TS-1 raw powder. Mix 100g of raw powder and 2g of Tianqing powder evenly, add 38g of silica sol and mix evenly, then extrude with extruder, dry the formed sample at 100°C for 12h, and then roast to obtain strip-shaped titanium-silicon molecular sieve TS- 1.

[0071] The XRD spectrum of titanium silicon molecular sieve TS-1 is attached figure 1 , 99% crystallinity.

Embodiment 2

[0072] The preparation of embodiment 2 titanium silicon molecular sieve Ti-MWW

[0073] Using boric acid as the boron source, silica sol (with a silica content of 30wt%) as the silicon source, and piperidine as the template, the mass ratio of boric acid, silica sol, and piperidine is 20:53:27, crystallized at 100°C After 30 hours, B-MWW was obtained after filtration, washing and drying. After the B-MWW was treated with nitric acid with a mass fraction of 33% at 120°C to deboron, the secondary hydrothermal crystallization was performed using tetrabutyl titanate as the titanium source. , crystallized at 160°C for 60 hours, filtered, washed, dried, and roasted to obtain the original titanium-silicon molecular sieve Ti-MWW powder. After mixing 38g of the original powder and 2g of Tianqing powder, add 38g of silica sol and mix evenly before extruding Machine extruded rods were formed, and the formed samples were dried at 100°C for 12 hours and then calcined to obtain strip-shaped t...

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Abstract

The invention provides a preparation method of glycolide. According to the preparation method of the glycolide, gaseous glycolate is subjected to a cyclization reaction under the catalytic condition of a titanium-containing molecular sieve, and the product glycolide is obtained. The preparation method provided by the invention has the advantages of mild reaction conditions and high product yield, can be continuously carried out, and does not need the participation of high vacuum and high-boiling-point solvents.

Description

technical field [0001] The invention belongs to the field of catalytic reactions, and in particular relates to a preparation method of glycolide. Background technique [0002] Environmental pollution (ie, "white pollution") caused by the uncontrolled mass production of non-degradable petroleum-based plastics and the abuse of disposable disposable petroleum-based plastic products has aroused serious concern worldwide. Biodegradable polymers based on renewable raw materials have achieved many important applications in the biomedical field, such as controlled release drug carriers, absorbable surgical sutures, implantable hard tissue repair materials, etc., and can be used as environmentally friendly materials for Manufacture of agricultural films, packaging materials, disposable sanitary products, disposable catering supplies, etc. [0003] Polyglycolic acid (PGA) is the simplest linear aliphatic polyester and the earliest commercially absorbable polymer material in vivo. Du...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D319/12B01J29/89B01J29/70C08G63/08C08G63/78
CPCC07D319/12C08G63/08C08G63/78B01J29/89B01J29/7057B01J29/7049B01J2229/183
Inventor 孙红影李进王炳春王贤彬
Owner CHINA CATALYST HLDG CO LTD
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