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Preparation method of UV curable organosilicon resin for direct writing molding

A technology of direct writing molding and silicone, which is applied in the direction of additive processing, etc., can solve the problems affecting the curing reaction speed of silicone resin, the resin performance of curing precision, the introduction of restricted reaction end groups, and poor compatibility, so as to improve the chemical phase. Low capacitive, meet the effect of direct writing molding, fast molding and curing

Active Publication Date: 2018-07-10
LASER FUSION RES CENT CHINA ACAD OF ENG PHYSICS
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the most reported silicone resin is acrylated polysiloxane prepolymer. Due to the poor compatibility between silicone resin and other resins, it is easy to separate phases when acrylate groups are introduced, which greatly limits the The introduction of reactive end groups; in addition, acrylate-based silicone resins are easily affected by oxygen resistance during UV curing, thus affecting the curing reaction speed, curing accuracy and resin properties of silicone resins

Method used

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  • Preparation method of UV curable organosilicon resin for direct writing molding
  • Preparation method of UV curable organosilicon resin for direct writing molding
  • Preparation method of UV curable organosilicon resin for direct writing molding

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 2

[0039] Step 1. Dissolve 20 g of hydroxyl-terminated siloxane resin and 5 g of methacryloxypropyltrimethylsilane (20.1 mmol) in 50 mL of 1,4-dioxane, stir until completely dissolved, and add 286 μL of concentrated Hydrochloric acid (0.4mmol), 362μL deionized water (20.1mmol), through N 2 protection, stirred and hydrolyzed at 20°C, and reacted for 12 hours to obtain a siloxane solution;

[0040] Step 2. Dissolve 1g of glycidyl ether methyl silsesquioxane (POSS) and 1g of hydroxypropyl acrylate in 20mL of 1,4-dioxane, add 20mg of N,N-dimethylbenzylamine, 1mg Hydroquinone, through N 2 protection, heating in an oil bath at 100°C, and reacting for 6 hours to obtain an acrylate-modified POSS intermediate;

[0041] Step 3, 1 mL of the acrylate-modified POSS intermediate 2 (0.1 g) prepared in step 2 was added dropwise to the siloxane solution (containing 5 g of reaction product siloxane) obtained in 5 mL of step 1. Stir and hydrolyze at 10°C for 2 hours, then raise the temperature t...

Embodiment 3

[0045] Step 1. Dissolve 20 g of alkoxy-terminated siloxane resin and 5 g of methacryloxypropyltrimethylsilane (20.1 mmol) in 25 mL of 1,4-dioxane, and stir at 70 rpm until completely dissolved. 286 μL concentrated hydrochloric acid (0.2 mmol), 362 μL deionized water (20.1 mmol) were added. Introduce N2 protection, stir and hydrolyze at 20°C, and react for 12 hours to obtain a siloxane solution;

[0046] Step 2: Add 1g of glycidyl ether methyl silsesquioxane (POSS) and 1g of hydroxyethyl methacrylate to 20mL of 1,4-dioxane, stir at 90rpm until completely dissolved, then add 20mg of triphenyl Based phosphine, 1mg p-benzoquinone, passed through N 2 protection, heating in an oil bath at 100°C, and reacting for 6 hours to obtain an acrylate-modified POSS intermediate;

[0047] Step 3, the acrylate-modified POSS intermediate (0.1g) prepared in 1mL step 2 was added dropwise in the siloxane solution (containing reaction product siloxane 10g) obtained in 10mL step 1, in 10 Stir and ...

Embodiment 4

[0051] Step 1. Dissolve 20 g of hydroxyl-terminated siloxane resin and 5 g of methacryloxypropyltrimethylsilane (20.1 mmol) in 50 mL of ethylene glycol dimethyl ether, stir at 70 rpm until completely dissolved, and add 286 μL of concentrated Hydrochloric acid (0.4mmol), 362μL deionized water (20.1mmol), through N 2 protection, stirred and hydrolyzed at 10°C, and reacted for 16 hours to obtain a siloxane solution;

[0052] Step 2. Add 0.5g glycidyl ether methyl silsesquioxane (POSS) and 1g pentaerythritol triacrylate to 5mL ethylene glycol dimethyl ether, stir at 60rpm until completely dissolved, then add 20mg tetramethyl bromide Ammonium chloride, 1mg p-methoxyphenol, passed through N 2 protection, heating in an oil bath at 100°C, and reacting for 6 hours to obtain an acrylate-modified POSS intermediate;

[0053] Step 3, the acrylate-modified POSS intermediate (0.3g) prepared in 1mL step 2 was added dropwise to the siloxane solution (containing 10g of reaction product siloxa...

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Abstract

The invention discloses a preparation method of a UV curable organosilicon resin for direct writing molding. The method includes: (1) employing hydroxyl terminated siloxane, alkoxy silane acrylate andother reactants to prepare a siloxane solution; (2) using epoxy modified POSS, hydroxyl acrylate and other reactants to prepare an acrylate modified POSS intermediate; (3) employing the prepared acrylate modified POSS intermediate and siloxane solution to prepare POSS modified organosilicon resin; and (4) adding a photoinitiator into the POSS modified organosilicon resin, conducting ultrasonic oscillation, and after the photoinitiator is completely dissolved and dispersed into the whole system, reducing the pressure to remove the solvent, thus obtaining the UV curable organosilicon resin fordirect writing molding. The preparation method of the rapid UV curable organosilicon resin for direct writing molding provided by the invention has the advantages of simple process, environmental friendliness, quick molding and curing and the like, can meet the needs of direct writing molding, and provides a new idea for modification of UV curable organosilicon resin.

Description

technical field [0001] The invention relates to the technical field of photocurable materials, in particular to a method for preparing a UV photocurable silicone resin for direct writing molding. Background technique [0002] Direct writing molding is an additive manufacturing method in which slurry is extruded and stacked layer by layer according to a pre-designed structure and molding path until the entire three-dimensional structure is formed. This technology has many advantages such as high manufacturing efficiency, low cost, wide application range of materials, and simple post-processing. The slurry used for direct writing molding mainly uses thermal curing or light curing to achieve rapid prototyping, in which ultraviolet light (UV) is used to trigger polymerization and cross-linking of polymer materials, which can instantly form solid materials, which can replace high energy consumption. , Thermosetting reaction process with long reaction time. [0003] Silicone res...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/20C08G77/06C08G77/14C08G77/16B33Y70/00
CPCB33Y70/00C08G77/045C08G77/06C08G77/14C08G77/16C08G77/20
Inventor 李婧张帅陈素芬彭倩玉李洁刘梅芳尹强李波
Owner LASER FUSION RES CENT CHINA ACAD OF ENG PHYSICS
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