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Siloxane bridging ladder polysiloxane, its preparation method and application

A technology of polysiloxane and siloxane bridge, which is applied in the field of siloxane bridge-based trapezoidal polysiloxane, which can solve the problems of temperature resistance, low adjustable degree of refractive index, and inconvenient industrial application.

Active Publication Date: 2021-02-23
ETERNAL CHINA INVESTMENT +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, because the siloxane bridging ladder polysiloxane is a homopolymer, there is a singleness of the main chain functional group structure, and its degree of polymerization, mechanical strength, temperature resistance and refractive index are relatively low in adjustability. problem, which brings inconvenience to its industrial application

Method used

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  • Siloxane bridging ladder polysiloxane, its preparation method and application
  • Siloxane bridging ladder polysiloxane, its preparation method and application
  • Siloxane bridging ladder polysiloxane, its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0280]

[0281] 1,1,5,5-tetramethoxy-1,5-diphenyl-3,3-diphenyltrisiloxane (274.4g, 0.5mol), 1,1,5,5-tetra Methoxy-1,5-bis(3-methacryloyloxypropyl)-3,3-diphenyltrisiloxane (324.5g, 0.5mol) and tetrahydrofuran (50mL) were placed under mechanical stirring 1. In a three-necked flask with a constant pressure dropping funnel, add DBU (1,8-diazabicyclo[5.4.0]undec-7-ene, 1.0 mL) and water (90 mL) under stirring at room temperature. The reaction was carried out at room temperature for 16 hours, then washed with dilute acid until neutral, concentrated, and purified by vacuum drying to obtain the siloxane bridging ladder polysiloxane with the structure shown above, wherein R 1 = R 2 = phenyl, R 3 = R 4 = 3-methacryloyloxypropyl, A 1 =A 2 =A 3 =A 4 = phenyl, Z 1 = Z 2 = Z 3 = Z 4 = hydrogen, m=1, x / y=1, z=0. The yield of the obtained siloxane bridging ladder polysiloxane random copolymer was 92%.

[0282] The resulting siloxane bridging ladder polysiloxane random copolyme...

Embodiment 2

[0284] 1,1,5,5-tetramethoxy-1,5-dimethyl-3,3-diphenyltrisiloxane (212.3g, 0.5mol), 1,1,5,5-tetra Methoxy-1,5-divinyl-3,3-diphenyltrisiloxane (224.3g, 0.5mol) and tetrahydrofuran (50mL) were placed in a three-neck flask with mechanical stirring and a constant pressure dropping funnel , and stirred at room temperature, DBN (1,5-diazabicyclo[4.3.0]non-5-ene, 0.9 mL) and water (90 mL) were added. The reaction was carried out at room temperature for 16 hours, then washed with dilute acid to neutrality, concentrated and vacuum-dried for purification to obtain the siloxane bridging ladder polysiloxane random copolymer of the structure of the aforementioned formula (II), wherein R 1 = R 2 = methyl, R 3 = R 4 = Vinyl, A 1 =A 2 =A 3 =A 4 = phenyl, Z 1 = Z 2 = Z 3 = Z 4 = Hydrogen, m=1, mean value of x+y is 14, x / y=1, z=0.

[0285]

[0286] The obtained siloxane bridging ladder polysiloxane random copolymer was a colorless transparent solid with a yield of 87%. The refrac...

Embodiment 3

[0288] 1,1,5,5-tetramethoxy-1,5-dimethyl-3,3-diphenyltrisiloxane (212.3g, 0.5mol), 1,1,5,5-tetra Methoxy-1,5-divinyl-3,3-diphenyltrisiloxane (224.3g, 0.5mol), 1,1,5,5-tetramethoxy-1,5-diphenyl Diphenyl-3,3-diphenyltrisiloxane (274.4g, 0.5mol) and tetrahydrofuran (50mL) were placed in a three-necked flask with mechanical stirring and a constant pressure dropping funnel, and under stirring at room temperature, potassium tert-butoxide was added (0.2g), water (135mL). The reaction was carried out at room temperature for 16 hours, then washed with dilute acid to neutrality, concentrated and vacuum-dried for purification to obtain the siloxane bridging ladder polysiloxane random copolymer of the structure of the aforementioned formula (II), wherein R 1 = R 2 = methyl, R 3 = R 4 = Vinyl, R 5 = R 6 = phenyl, A 1 =A 2 =A 3 =A 4 =A 5 =A 6 = phenyl, Z 1 = Z 2 = Z 3 = Z 4 =hydrogen, m=1, its molecular weight was analyzed by VPO (vapor pressure osmometer) test, and the aver...

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Abstract

A siloxane-bridged ladder polysiloxane, having a main structural framework as represented by formula I, wherein the definitions of each substituent, m, x, y, and z are as stated in the description and the claims. The present invention also relates to a siloxane-bridged ladder polysiloxane random / block copolymer, and a graft copolymer prepared by a siloxane-bridged ladder polysiloxane formulation. The siloxane-bridged ladder polysiloxane retains the specific temperature resistance, flexibility, and good compatibility with general-purpose polymers of siloxane-bridged ladder polysiloxane fragments, and the degree of polymerization, mechanical strength, temperature resistance, optical properties, and the like can be adjusted according to different compositions and proportions of copolymerized fragments, the compositions and proportions of end-capping agents, and different structures of graft units, and the like.

Description

technical field [0001] The invention relates to a siloxane bridging ladder polysiloxane, its preparation method and application. Background technique [0002] Ladder polymer is a ribbon-shaped macromolecule formed by connecting two or more single chains. Compared with ordinary single-chain polymers, this type of polymer has good solubility, temperature resistance, and chemical and biological stability. and high mechanical properties. When random fragmentation occurs under the influence of external factors, the chance of simultaneous fragmentation of two single chains connected on the same ladder strut is very small, and as the molecular weight (or degree of polymerization) increases, the chance of such fragmentation is even smaller. At the same time, due to the unique temperature resistance, weather resistance, radiation resistance, low surface tension, high gas permeability and electrical insulation properties of silicon-containing polymers, trapezoidal silicone polymers h...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/20C08G77/14C08G77/06C08G77/12C08G77/26C08G77/24C08G77/28C08G77/44C08G77/458C08G77/46
CPCC08G77/06C08G77/12C08G77/14C08G77/20C08G77/24C08G77/26C08G77/28C08G77/44C08G77/458C08G77/46C08G77/80
Inventor 曹菁潘赏张榕本方世壁
Owner ETERNAL CHINA INVESTMENT
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