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Hyper-branched polysiloxane containing macro-ring structure and synthetic method thereof

A technology of polysiloxane and synthesis method, which is applied in the field of hyperbranched polysiloxane synthesis, which can solve the problems of cumbersome crosslinking and synthesis process of synthesis technology, small pores between molecular branch chains, and cumbersome synthesis process, etc., and achieve product purification The process is simple and easy, the synthesis efficiency is high, and the effect of a wide range of applications

Active Publication Date: 2015-02-04
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, in the paper published by M. Miyasaka et al. on Polymer Journal (Polymer Journal, 2010, 42, 799-803), the four-membered ring structure and cage-shaped tetrasilanol synthesized from raw materials such as cyclic tetrasilanol and double deck tetrasilanol Hyperbranched polysiloxane composed of structural polysiloxane, this type of polysiloxane is easy to crosslink during synthesis, so its application range is also greatly limited
Another example is the article published by K.Wada et al. on Chemical communications (Chemical Communications, 2005, 95-97). They synthesized a hyperbranched polysiloxane composed of clathrate polysiloxane from clathrate polysiloxane. Polysiloxanes, but the synthesis process is cumbersome
[0003] In short, the existing hyperbranched polysiloxanes have the problem of too small pores between molecular branches, and the synthesis technology has the problems of easy crosslinking and cumbersome synthesis process.

Method used

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  • Hyper-branched polysiloxane containing macro-ring structure and synthetic method thereof
  • Hyper-branched polysiloxane containing macro-ring structure and synthetic method thereof
  • Hyper-branched polysiloxane containing macro-ring structure and synthetic method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0048] Preparation of Hyperbranched Polysiloxane Containing Macrocyclic Structure with Phenyl and Methyl Side Groups

[0049] At 80°C, add 80 grams of 1,1,3,3-tetramethyl-5,7-diphenylcyclotetrasilane and 0.08 grams of water into a 500-milliliter two-necked flask containing 0.008 grams of palladium chloride and 300 milliliters of tetrahydrofuran , and stir for 10 minutes. Activated carbon was added to remove palladium chloride, filtered, the solvent was evaporated with a rotary evaporator, and finally vacuum-dried to obtain a white solid with a yield of 85% and a branching degree of 90%.

[0050] The gel permeation chromatogram of hyperbranched polysiloxane containing macrocyclic structure with side groups of phenyl and methyl is as follows: figure 1 As shown, the infrared spectrum is shown in figure 2 As shown, the H NMR spectrum is shown as image 3 As shown, the NMR silicon spectrum is shown as Figure 4 As shown, the thermogravimetric spectrum is shown as Figure 5 sh...

Embodiment 2

[0052] Preparation of hyperbranched polysiloxane with methyl side group containing macrocyclic structure

[0053] -60°C, add 10 grams of 1,1,3,3,5,7-hexamethylcyclotetrasiloxane and 10 grams of water into a 100 ml two-necked flask containing 1 gram of nickel acetylacetonate and 50 ml of acetone, Stir for 24 hours. A chromatographic column filled with diatomaceous earth was used to remove nickel acetylacetonate, then the reaction solution was poured into 200 milliliters of methanol, solids were precipitated, filtered to obtain solids, and finally vacuum-dried to obtain white solids with a yield of 65% and a degree of branching of 70 %.

Embodiment 3

[0055] Preparation of macrocyclic hyperbranched polysiloxane with side groups cyclohexyl and vinyl

[0056] At 140°C, 100 grams of 1,3,3,5,7,7-hexacyclohexyl cyclotetrasiloxane, 100 grams of octavinyl cyclotetrasiloxane and 50 grams of water were added to 6 grams of ferrocene and 300 ml of cyclohexanone in a 500 ml two-neck flask, stirred for 10 hours. Remove ferrocene with a chromatographic column filled with aluminum oxide, then pour the reaction solution into 1000 milliliters of methanol, solids are precipitated, filtered to obtain solids, and finally vacuum-dried to obtain white solids, with a yield of 75% and a degree of branching of 80 %.

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Abstract

The invention relates to the technical field of a hyper-branched polysiloxane synthesis technology, specifically to hyper-branched polysiloxane containing a macrocycle structure and a synthetic method thereof. According to the synthetic method, small-ring siloxane and water which are used as raw materials are subjected to a combination reaction in an organic solvent under the action of a metal catalyst, and a reaction product undergoes post-treatment so as to prepare the hyper-branched polysiloxane containing a macrocycle structure. The synthetic method has advantages as follows: the reaction condition is mild; energy consumption is low; synthetic efficiency is high; crosslinking is not easy to happen during the synthetic process; and the product purification process is simple and practicable.

Description

technical field [0001] The invention relates to the technical field of hyperbranched polysiloxane synthesis, in particular to a hyperbranched polysiloxane containing a macrocyclic structure and a synthesis method thereof. Background technique [0002] Hyperbranched polysiloxane has important applications, such as molecular recognition, catalyst carrier, drug delivery system, high temperature resistant coating, etc. So far, there are mainly two types of hyperbranched polysiloxanes reported. The first kind of hyperbranched polysiloxane is a hyperbranched polysiloxane composed of single chains, such as the papers published in Journal of the American Chemical Society by people such as H.Uchida (Journal of the American Chemical Society, 1990, 112 , 7077-7079), using multifunctional silanes as raw materials to synthesize hyperbranched polysiloxanes composed of single chains. The pores formed between the branch chains of such hyperbranched polysiloxane molecules are too small, and...

Claims

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Application Information

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IPC IPC(8): C08G77/16
Inventor 李泽刘利锋吴春勇来国桥
Owner HANGZHOU NORMAL UNIVERSITY
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