A kind of preparation method and application of modified hnts supported tin-based catalyst

A catalyst, tin-based technology, applied in the field of preparation of modified HNTs supported tin-based catalysts, can solve the problems of limiting the application of polycaprolactone, impact, and insufficient thermal stability, and achieve the effect of improving the scope and degree of application

Active Publication Date: 2022-06-24
CHINA UNIV OF GEOSCIENCES (WUHAN)
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, polycaprolactone also has shortcomings. Thermal properties are very important for the processing and recycling of polymers. However, the temperature of polycaprolactone prepared by traditional tin-based catalysts is 215°C-230°C when it loses 1 wt%. Thermal stability is not good enough
This greatly affects and limits the application of polycaprolactone in biomedicine and daily necessities

Method used

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  • A kind of preparation method and application of modified hnts supported tin-based catalyst
  • A kind of preparation method and application of modified hnts supported tin-based catalyst
  • A kind of preparation method and application of modified hnts supported tin-based catalyst

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preparation example Construction

[0031] An embodiment of the present invention provides a method for preparing a modified HNTs-supported tin-based catalyst, with reference to Figure 8, which mainly includes the following steps:

[0032] S1, the stannous chloride (SnCl 2 ) and halloysite nanotubes (HNTs) were added to toluene, and stirred uniformly to obtain a first mixture, wherein, in parts by weight, the first mixture included 100 parts of toluene, 5-12 parts of halloysite nanotubes, 0.4-1.3 parts of stannous chloride; based on the natural multi-walled microtubule structure of HNTs, HNTs can act as a solid carrier when the monomer catalyzes polymerization. The active sites are enhanced by loading stannous chloride onto the inner and outer surfaces of the modified HNTs by physical force;

[0033] S2. Add silane coupling agent KH-550 (APTES) into toluene, stir evenly to obtain a second mixture, wherein, in parts by weight, the mixed solution includes 100 parts of toluene and 1-3 parts of silane coupling agen...

Embodiment 1

[0041] A preparation method of a modified HNTs-supported tin-based catalyst, which mainly comprises the following steps:

[0042] S1, the stannous chloride (SnCl 2 ) and halloysite nanotubes (HNTs) were added into toluene, and stirred uniformly to obtain a first mixture, wherein, in parts by weight, the first mixture included 100 parts of toluene, 8.2 parts of halloysite nanotubes, chlorinated 0.7 parts of tin;

[0043] S2, adding silane coupling agent KH-550 (APTES) into toluene, stirring evenly to obtain a second mixture, wherein, in parts by weight, the mixed solution includes 100 parts of toluene and 1.7 parts of silane coupling agent;

[0044] S3, with n((SnCl 2 ):n(APTES)=1:1 Add the second mixture prepared by S2 to the first mixture prepared by S1 to obtain the third mixture, and apply three nitrogen purge cycles, stir for 15h, stirring speed 500r / min , the modified HNTs-supported tin-based catalyst (APTES-P-HNTs-SnCl 2 ).

[0045] Taking the halloysite nanotubes i...

Embodiment 2

[0051] S1. The modified HNTs supported tin-based catalyst and ε-caprolactone prepared in Example 1 were mixed with a mass ratio m(APTES-P-HNTs-SnCl 2 ):m(ε-caprolactone)=1:100 ratio, put it into the reaction flask to form a mixture, add magnetron into the mixture, carry out end-capping operation after evacuating for 45min, and then put it into an oil bath, Start the magnetic stirrer and perform magnetic stirring to obtain the product, wherein the stirring speed is 500r / min, and after rising from room temperature to 150°C, the temperature is kept constant for 24h;

[0052] S2. Add dichloromethane to the product to completely dissolve the product, and finally add methanol to precipitate the product, stand, filter and dry to obtain PCL / HNTs with a yield of 92.4% and a number average molecular weight of 28190. Wherein, in terms of weight ratio, product:dichloromethane:methanol=1:2.65:100.

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Abstract

The present invention relates to the technical field of organic polymers, in particular to a preparation method and application of a modified HNTs supported tin-based catalyst. The method comprises the following steps: S1 2 ) and halloysite nanotubes (HNTs) were added to toluene, stirred uniformly to obtain the first mixture; S2 added silane coupling agent KH‑550 (APTES) to toluene, stirred uniformly to obtain the second mixture; S3 with n( SnCl 2 ):n(APTES)=1:1 ratio, the second mixture prepared by S2 is added to the first mixture prepared by S1 to obtain the third mixture, and three nitrogen cycles are applied, stirring for 12-24h, stirring speed 200-800r / min, can obtain described modified HNTs supported tin-based catalyst (APTES-P-HNTs-SnCl 2 ), where n is the amount of substance. The preparation method of the present invention is based on the natural multi-walled microtubule structure of HNTs, and the SnCl is loaded by physical force 2 To modify the inner and outer surfaces of HNTs, the active sites are enhanced, the catalytic performance is excellent, the organic compatibility is good, and it is also an excellent filler for the polymer matrix.

Description

technical field [0001] The invention relates to the technical field of organic macromolecular polymers, in particular to a preparation method and application of a modified HNTs-supported tin-based catalyst. Background technique [0002] Halloysite nanotubes (HNTs) are kaolinite-based minerals with a 1:1 dioctahedral structure and exhibit a multi-layered tubular structure that is chemically similar to kaolinite. On the one hand, halloysite nanotubes have high specific surface area, high aspect ratio, good dispersion and excellent mechanical properties, and thus are excellent fillers for polymer composites. The mechanical properties, thermal stability and flame retardancy of polymer composites obtained with halloysite nanotubes as fillers can be significantly improved. On the other hand, HNTs are widely used in the catalysis industry because their nano-scale tubular structure can immobilize catalysts on the surface or inside the tube, and has less barrier to the diffusion of ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/85C08G63/82C08G63/08C08K9/06C08K3/04
CPCC08G63/823C08G63/85C08G63/82C08G63/08C08K9/06C08K3/041
Inventor 杨刚马睿靳洪允杜文杰廖佩珊刘志研李耀
Owner CHINA UNIV OF GEOSCIENCES (WUHAN)
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