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Multi-arm siloxane bridge-based trapezoidal polysiloxane copolymer and preparation method and application thereof

A polysiloxane and siloxane bridge technology, applied in the field of polymers, can solve the problems of reducing the reactivity of reactive groups and the like

Active Publication Date: 2017-11-28
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to overcome the relatively rigid and relatively large steric hindrance of the molecular chain structure of the siloxane bridging ladder polysiloxane in the prior art, so that the reactive group reactivity of the side group or terminal group on the chain is reduced. problems, while improving its compatibility with general-purpose silicone resins and expanding its application range

Method used

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  • Multi-arm siloxane bridge-based trapezoidal polysiloxane copolymer and preparation method and application thereof
  • Multi-arm siloxane bridge-based trapezoidal polysiloxane copolymer and preparation method and application thereof
  • Multi-arm siloxane bridge-based trapezoidal polysiloxane copolymer and preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0094] Via triethoxysilane, diphenyldihydroxysilane, HO(MeHSiO) 100 H Preparation of Multi-Armed Siloxane Bridged Ladder Polysiloxane Copolymer.

[0095] (1) Under the protection of dry nitrogen, put 26ml (0.138 moles) of triethoxysilane and 20ml of tetrahydrofuran into a multi-necked flask equipped with a condenser tube and a dropping funnel; 10g (0.046 moles) of diphenyl Dihydroxysilane was dissolved in 20ml tetrahydrofuran, 1ml pyridine (0.0124 mol) was dissolved in 20ml tetrahydrofuran, and the two solutions were respectively placed in constant pressure dropping funnels; the solutions in the two constant pressure dropping funnels were dropped separately at -20°C Add it into a multi-neck flask, and stir; after the dropwise addition, continue to react for 2.5 hours; after stopping the reaction, distill and concentrate to remove ethanol and unreacted triethoxysilane and part of tetrahydrofuran to obtain a pure intermediate solution; adding tetrahydrofuran to the intermediate...

Embodiment 2

[0102] Z prepared in Example 1 1 = Z 2 = Z 3 = Z 4 The multi-arm siloxane bridging ladder polysiloxane copolymer of = H (I 1 ) with 1,1,3,3-tetramethyldisiloxane to further react to obtain multi-arm siloxane bridging ladder polysiloxane copolymer (II 1 ).

[0103] At 60°C, to the multi-arm siloxane bridging ladder polysiloxane copolymer prepared in Example 1 (I 1 ) into 0.3 g (2.2×10 -3 mol), 0.025 g (2.2×10 -4 ) sulfuric acid, 20ml tetrahydrofuran, after reacting for 7 hours, heat up to 120°C to distill tetrahydrofuran and water; then filter and separate the reaction mixture, collect the clear liquid, wash with water until neutral, concentrate, and dry under reduced pressure for purification to obtain formula (I) The shown multi-arm siloxane bridging ladder polysiloxane copolymer (II 1 ), where E 1 =E 2 = H, A 1 =A 2 = phenyl, B 1 =B3 =B 5 =B 7 = methyl, B 2 =B 4 =B 6 =B 8 = H, Z 1 = Z 2 = Z 3 = Z 4 =SiHMe 2 , Me=methyl, m=1, n=20, L=1, k 1 =k 2 =k ...

Embodiment 3

[0107] Through phenyltrimethoxysilane, diphenyldihydroxysilane, HO(Me 2 SiO) 243 H Preparation of Multi-Armed Siloxane Bridged Ladder Polysiloxane Copolymer.

[0108] (1) Under the protection of dry nitrogen, put 50ml (0.68 moles) of phenyltrimethoxysilane in a multi-necked flask equipped with a condenser tube and a dropping funnel, and dissolve 10 grams (0.046 moles) of phenyltrimethoxysilane at -20°C ) The mixed solution of diphenyldihydroxysilane and 50 grams of tetrahydrofuran was added dropwise into the multi-neck flask through the dropping funnel, and ammonia gas was introduced at the same time; after the dropwise addition, the ammonia gas flow was stopped, and the temperature was gradually raised to 70°C for 1 hour reaction To remove ammonia; after stopping the reaction, distill and concentrate to remove methanol, unreacted phenyltrimethoxysilane and part of tetrahydrofuran to obtain a pure intermediate solution; mix the intermediate solution with toluene to obtain a c...

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Abstract

The invention relates to a multi-arm siloxane bridge-based trapezoidal polysiloxane copolymer and a preparation method and an application thereof. The copolymer is prepared by performing a copolymerization reaction on siloxane bridge-based trapezoidal polysiloxane and a precursor F1O(P1P2SiO2)kF2 of single chain polysiloxane. The middle part of the copolymer retains the rigidity of the siloxane bridge-based trapezoidal polysiloxane, and the flexibility and the compatibility with other universal organic silicon resin are enhanced in the presence of a flexible multi-arm structure, so that the copolymer is a rigid and flexible material. Meanwhile, based on the special structural design of the copolymer, the influence on end group or side chain reactive groups by the rigidity and steric effect of the molecular chain is reduced, so that other organic silicon resin or polymers are further favorably modified by means of chemical reactions.

Description

technical field [0001] The invention relates to a polysiloxane copolymer, in particular to a multi-arm siloxane bridging ladder polysiloxane copolymer and its preparation method and application, belonging to the technical field of polymers. Background technique [0002] Polysiloxane has excellent high and low temperature resistance, radiation resistance, good biocompatibility and stability, so it has a wide range of applications in various fields such as aerospace, electronic devices, and biomedicine. Through M in the molecular chain (ie: R stands for side group), D (ie: R stands for side group), T (ie: R represents the side group), Q (ie: ) content and side groups can adjust its performance in a wide range. [0003] Ladder polysiloxane is a polysiloxane with double-chain or multi-chain and ladder-like molecular structure. Compared with the corresponding single-chain polysiloxane macromolecule, it has better high temperature resistance, Radiation, weather resistance...

Claims

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Application Information

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IPC IPC(8): C08G77/16C08G77/20C08G77/24C08G77/28C08G77/14C08L83/06C08L83/07
CPCC08G77/14C08G77/16C08G77/20C08G77/24C08G77/28C08J5/18C08J2383/06C08J2483/06C08L83/06C08L2203/16C08L2205/025
Inventor 曹新宇尚欣欣汪洁马永梅段珊张榕本方世璧
Owner INST OF CHEM CHINESE ACAD OF SCI
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