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A kind of high refractive index organosilicon resin and preparation method thereof

A high refractive index, silicone technology, applied in the field of silicone materials, can solve the problems of increased resin density, high resin density, reduced impact resistance, etc., to reduce odor, improve productivity, and prevent ring opening.

Active Publication Date: 2021-04-13
SHENZHEN ANPIN SILICONE MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] (1) The introduction of aromatic compounds or condensed ring compounds can increase the refractive index, but the prepared polymer has large dispersion, and there are hard and brittle defects in mechanical properties, and the refractive index can only reach about 1.5
[0006] (2) Introduce halogen elements other than F, but the density of the resin increases, the weather resistance is poor, and it is easy to yellow
[0007] (3) Introduce heavy metal ions such as lead, lanthanum or TiO 2 , PbS, FeS nanoparticles to increase the refractive index, but the resin density is high, the impact resistance is reduced, it is easy to yellow, and the practicability is poor
[0010] However, the existing method of introducing sulfur through sulfur heterocyclic monomers is prepared by Grignard reaction under ultra-low temperature conditions, which has the disadvantages of strong product odor and harsh preparation conditions, which limits the application of such high refractive index silanes and resins to promote

Method used

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  • A kind of high refractive index organosilicon resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Add ethyl acetate (382.45g), ethanol (191.23g), 1,3-dithiapentane-2-ylmethanol into a four-necked flask equipped with a condenser, nitrogen inlet and constant pressure funnel (108.99g, 0.80mol) and ethyl orthosilicate (208.33g, 1.00mol) were stirred for 40min, after 1,3-dithiapentane-2-ylmethanol was completely dissolved, dichloroacetic acid (3.27g, 0.0254mol) was added , Trifluoromethanesulfonic acid (2.29g, 0.0153mol) was stirred for 10min, water (36.00g, 2mol) was added dropwise into the reaction system at a rate of 5 drops / min in a constant pressure funnel, and after reacting at 90°C for 48h, adding Vinyldimethylethoxysilane (ViMe 2 SiOEt) (65.13g, 0.5mol), reflux at 100°C for 24h, cool to room temperature, add ammonium bicarbonate (4.18g, 0.0538mol) and stir for 10min, separate the oil layer and decompress at 30°C, -0.095MPa Distilled for 20 minutes, added ethyl acetate (382.45g), then added petroleum ether (114.74g) to break the emulsification, washed with deion...

Embodiment 2

[0047] Add benzene (819.72g), isopropanol (245.92g), 1,3-dithiane-2-carboxylic acid into a four-neck flask equipped with a condenser tube, nitrogen inlet and constant pressure funnel (164.25g, 1.00mol) and ethyl orthosilicate (208.33g, 1.00mol), after stirring for 60min, after 1,3-dithiane-2-carboxylic acid was completely dissolved, 2-propiolic acid (8.21g, 0.1173mol), 37%wt concentrated hydrochloric acid (4.10g, 0.0415mol), stirred for 30min, added distilled water (54.00g, 3mol) into the reaction system dropwise at a rate of 7 drops / min in a constant pressure funnel, and reacted at 100°C 24h, add tetramethyldiethylenedisiloxane (ViMe 2 SiOSiMe 2 Vi) (37.28g, 0.2mol), reflux at 95°C for 15h, cool to room temperature, add ammonium bicarbonate (15.07g, 0.1906mol) and stir for 20min, separate the oil layer, decompress at 35°C, -0.095MPa Distill for 20 minutes, add n-hexane (532.82g), then add petroleum ether (204.93g) to break the emulsification, wash with deionized water unti...

Embodiment 3

[0049] Add cyclohexane (1264.37g), tetrahydrofuran (337.17g), 4-(1,3-dithiolane)phenol into a four-neck flask equipped with a condenser tube, nitrogen inlet and constant pressure funnel (237.97g, 1.2mol) and methyl orthosilicate (152.22g, 1.00mol) were stirred for 50min, after 4-(1,3-dithiolane) phenol was completely dissolved, trichloroacetic acid (19.04g, 0.1165mol) was added ), 98%wt concentrated sulfuric acid (3.37g, 0.0337mol) was stirred for 30min, and distilled water (54.00g, 3mol) was added dropwise in the reaction system at a rate of 10 drops / min in a constant pressure funnel, and after reacting for 36h at 100°C, Add dimethylethoxysilane (31.27g, 0.3mol), reflux at 90°C for 12h, cool to room temperature, add ammonium bicarbonate (20.36g, 0.2575mol) and stir for 30min. Distill under reduced pressure at -0.095MPa for 20min, add ethyl acetate (632.19g), then add ether (210.73g) to break the emulsification, wash with deionized water until neutral, separate the oil layer,...

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Abstract

The invention discloses a high-refractive-index silicone resin and a preparation method thereof. The high-refractive-index silicone resin has an average composition formula: (R 1 SiO 3 / 2 ) a (R 1 2 SiO) b (SiO 2 ) c (R 1 3 SiO 1 / 2 ) d (R 2 R 3 R 4 SiO 1 / 2 ) e , the R 1 has the structural formula ‑OR 0 , the R 0 Containing sulfur-containing heterocyclic groups, the resin is prepared by an improved preparation method, which can significantly improve the stability of the sulfur-containing heterocyclic groups during the synthesis process, so that the prepared resin has low odor and good compatibility with silicone resins. Moreover, the preparation conditions are mild and the process is simple.

Description

technical field [0001] The invention belongs to the technical field of organic silicon materials, and relates to a high refractive index organic silicon resin and a preparation method thereof. [0002] technical background [0003] The application fields of optical materials are expanding, and the products are constantly developing towards high refractive index, high light transmittance and high reliability. Silicone materials are widely used in medicine, biology because of their good temperature resistance, mechanical properties and non-toxic environmental protection. , communications and other optical material preparation fields have been widely used. At present, silicone materials used in optical lenses, optical fiber materials and other fields require a higher refractive index, even as high as 1.7 or more, and have good mechanical properties. [0004] The prior art methods for improving the refractive index of silicone materials are mainly to introduce high refractive in...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/28C08G77/06
CPCC08G77/06C08G77/28
Inventor 刘珠祝琳丁小卫
Owner SHENZHEN ANPIN SILICONE MATERIAL