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Photocuring material and application thereof

A photocurable material, hyperbranched technology, applied in the direction of coating, can solve the problem of no report, etc., and achieve the effect of high crosslinking density, high wear resistance and chemical resistance, and good thermal stability.

Active Publication Date: 2016-05-25
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, up to now, there are only few literatures about the UV curing of hyperbranched polycarbosilane, and only study its UV curing kinetics, and the influence of light intensity, temperature, etc. on its conversion rate and curing rate, but not It is reported that hyperbranched polycarbosilane is used as a photosensitive resin for photocurable 3D printing materials

Method used

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  • Photocuring material and application thereof
  • Photocuring material and application thereof
  • Photocuring material and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Step 1: Synthesis of vinyl-containing hyperbranched polycarbosilane

[0031] References (Chinese Chemical Letters, 2007, 18, 754-757.) to synthesize vinyl-containing hyperbranched polycarbosilane, the specific steps are: adding magnesium chips (1.04mol) to CH 2 =CHCH 2 Cl(0.12mol), Cl 3 SiCH 2 Cl (0.46mol) and Cl 2 Si(CH 3 )CH 2 Cl (0.23mol) in tetrahydrofuran (200mL) was reacted at 60°C for 12 hours, then lithium aluminum hydride (0.37mol) was added in an ice-water bath, and the reaction was continued at 60°C for 12 hours. After the reaction finished, the reaction solution was poured into the aqueous hydrochloric acid solution with a concentration of 4mol / L and stirred. After stirring for 2 hours, n-hexane (500mL) was added to the water, the layers were static, the organic phase was separated and dried with sodium sulfate, and finally Dry in vacuum at 60°C to obtain vinyl-containing hyperbranched polycarbosilane. The synthetic route is as follows (it should be n...

Embodiment 2

[0039] Step 1: Synthesis of acryloxy-containing hyperbranched polycarbosilane

[0040] References (Chinese Chemical Letters, 2007, 18, 754-757.), synthesis of hyperbranched polycarbosilane containing Si-Cl bonds, and then refer to literature (Polymer, 2006, 47, 1519–1525), to obtain hyperbranched polycarbosilane containing acryloyloxy groups Polycarbosilane, the specific steps are: adding magnesium chips (1.0mol) to the CH 3 CH 2 CH 2 Cl (0.20mol), Cl 3 SiCH 2 Cl (0.15mol), Cl 2 Si(CH 3 )CH 2 Cl (0.45mol) in tetrahydrofuran (200mL) was reacted at 60°C for 12 hours, then 2-hydroxyethyl acrylate (0.6mol) and pyridine (0.6mol) were added in an ice-water bath and reacted for 1.5 hours. After the reaction finishes, remove the insolubles by filtration, pour the filtrate into an aqueous hydrochloric acid solution with a concentration of 4mol / L and stir, after stirring for 2 hours, add n-hexane (500mL) to the water, separate the organic phases and use sulfuric acid Sodium dryi...

Embodiment 3

[0050] Step 1: Synthetic vinyl-containing hyperbranched polycarbosilane with reference to Example 1

[0051] Step 2: Preparation of photocurable materials

[0052] The formula of light-curing material is: hyperbranched polycarbosilane (82wt%) containing vinyl, active diluent tripropylene glycol diacrylate (10wt%), ultraviolet photoinitiator 1-hydroxycyclohexyl phenyl ketone ( 4wt%) and benzophenone (3.6wt%), co-initiator CN373 (0.4wt%). The above raw materials were mixed under light shielding and mechanically stirred at room temperature for 2 h.

[0053] Step 3: Light Curing 3D Printing

[0054] The above-mentioned light-curing material in the working chamber of the nozzle quickly forms small droplets, and then sprays onto the support material at a certain speed and frequency, and solidifies under the action of ultraviolet light (the light source is a 600W medium-pressure mercury lamp). Form a three-dimensional structure. After characterization, the Shore hardness is 86HD,...

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Abstract

The invention relates to a photocuring material which comprises the following components in percentage by weight: 60-98% of hyperbranched polycarbosilane, 0-35% of active diluent, 0.1-8% of photoinitiator and 0-10% of additive, wherein the hyperbranched polycarbosilane contains an unsaturated double bond, and the number-average molecular weight of the hyperbranched polycarbosilane is 300-15,000; the unsaturated double bond is acryloyloxy, methylacryloyloxy, vinyl or allyl; and the content of the unsaturated double bond in the hyperbranched polycarbosilane is 1-30% by weight. The invention also relates to an application of the photocuring material in photocuring 3D printing and an application in preparation of a SiC component. The photocuring material provided by the invention has relatively low viscosity and is convenient to spray out of a nozzle of 3D printing equipment while the curing speed is high and the shrinkage rate in curing is little.

Description

technical field [0001] The invention relates to the field of curing materials, in particular to a light curing material and its application. Background technique [0002] 3D printing can quickly manufacture components of any complex shape, without molds, produces very little waste, is simple to operate, fast in molding speed, pollution-free in the molding process, and has obvious cost and efficiency advantages in non-batch production. It has become a research hotspot of current rapid prototyping technology. The forming principle of light-curing 3D printing technology is to use liquid light-curing materials to rapidly polymerize under light irradiation, and the light-curing materials quickly change from liquid to solid. [0003] Photocurable materials for photocurable 3D printing generally consist of photosensitive resins, reactive diluents (reactive monomers), photoinitiators and additives. The Chinese invention patent (CN104559196A) discloses a colorless and transparent l...

Claims

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Application Information

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IPC IPC(8): C08F283/00C08F222/20C08G77/60C09D183/16C09D7/12C04B35/565C04B35/622
CPCC09D7/61C09D7/65C09D183/16C04B35/565C04B35/622C08F283/00C08G77/60C04B2235/6026C08L83/04C08K3/34C08F222/1025C08F222/102
Inventor 何流裴学良季鹏苗玉龙杨建行黄庆
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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