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Preparation method of light-cured resin containing silicon nano gel for 3D printing and application of light-cured resin

A technology of silicon nanogel and photocurable resin, which is applied in the direction of additive processing, etc., can solve the problems of large resin shrinkage and large reaction stress, and achieve the effects of reducing resin shrinkage, small volume shrinkage, and mild reaction conditions

Inactive Publication Date: 2016-11-23
CHANGZHOU HUAKE POLYMERS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to solve the problem of large reaction stress in the resin photocuring process and large resin shrinkage after curing in the prior art, and provide a preparation method and application of silicon-containing nanogel photocurable resin for 3D printing

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Prepare high-precision silicon-containing photocurable resin according to the following raw material formula and preparation method.

[0030] Add 1.27g of vinyl silicone oil, 6.61g of isobornyl methacrylate, 0.079g of cyclohexanone peroxide, dibenzoyl peroxide and 0.20g of mercaptoethanol into a 500ml three-necked flask, add 15.842g of ethyl acetate, at 90 ℃, under the condition of nitrogen protection, after magnetic stirring for 2 hours, the temperature was lowered, and the solution in the reaction kettle was settled twice with 306.80 g of n-hexane to remove unreacted monomers. After the obtained polymer was dissolved in 40 g of dichloromethane, the solvent was removed by distillation under reduced pressure to obtain nanogel particles with hydroxyl groups. The obtained nanogel particles with hydroxyl are dissolved in anhydrous dichloromethane, add 0.36g (2.31mmol) IEM, add dropwise 0.10g DBTDL, react under nitrogen protection conditions at room temperature, until Fouri...

Embodiment 2

[0032] Add 1.90g styrene silicone oil, 20.9g methyl acrylate, 0.418g azobisisobutyronitrile, azobisisovaleronitrile, 1.25g mercaptoacetic acid into a 500ml three-necked flask, add 105.6g ethyl acetate at 95°C, nitrogen Under protective conditions, after magnetic stirring for 3 hours, the temperature was lowered, and 301.92 g of the solution in the reactor was settled twice with n-hexane to remove unreacted monomers. After the obtained polymer was dissolved in 40 g of dichloromethane, the solvent was removed by distillation under reduced pressure to obtain nanogel particles with hydroxyl groups. The obtained nanogel particles with hydroxyl are dissolved in anhydrous dichloromethane, add 0.36g (2.31mmol) IEM, add dropwise 0.10g DBTDL, react under nitrogen protection conditions at room temperature, until Fourier transform infrared spectrometer detects no to hydroxyl. The product was then purified as previously described.

Embodiment 3

[0034] Add 2.53g of acryloyl silicone oil, 13.92g of ethyl acrylate, 0.42g of cyclohexanone peroxide, azobisisobutyronitrile, and 1.11g of mercaptopropanol and mercaptopropionic acid into a 500ml three-necked flask, and add 80.74g of butyl acetate , Benzene, at 80° C., under the condition of nitrogen protection, after magnetic stirring for 5 hours, the temperature was lowered, and 295.04 g of the solution in the reaction kettle was settled twice with n-hexane to remove unreacted monomers. After the obtained polymer was dissolved in 40 g of dichloromethane, the solvent was removed by distillation under reduced pressure to obtain nanogel particles with hydroxyl groups. The obtained nanogel particles with hydroxyl groups are dissolved in anhydrous dichloromethane, 0.36g (2.31mmol) IEM is added, 0.10g DBTDL is added dropwise, and reacted under nitrogen protection conditions at room temperature until the Fourier infrared spectrometer detects no hydroxyl. The product was then purif...

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Abstract

The invention relates to light-cured resin, in particular to a preparation method of light-cured resin containing silicon nano gel for 3D printing and application of the light-cured resin. According to the resin, acrylate monomer and acrylic ester are used for modifying organo-siloxane, solution free radical polymerization is used for preparing organic silicon nano gel, the organic silicon nano gel of different structures, molecular weight and particle sizes is prepared by adjusting the structures and proportion of the monomer and organosilicone, and the optimal structure and proportion of the organic silicon nano gel are obtained. The light-cured resin with excellent comprehensive performance and containing the silicon nano gel for 3D printing is obtained by regulating the composition and proportion of the light-cured resin, and the light-cured resin has the advantages that the processing is easy, the water resistance is good, the volume shrinkage is small, and the material accuracy is high.

Description

technical field [0001] The invention relates to a photocurable resin, in particular to a preparation method and application of a silicon-containing nanogel photocurable resin for 3D printing. Background technique [0002] Photosensitive resin is UV photocurable resin, which is composed of prepolymer and monomer, and photoinitiator (or photosensitizer) is added to it, which can immediately cause polymerization reaction and complete curing under the irradiation of ultraviolet light (250-300nm) of a certain wavelength. . Photosensitive resin is generally liquid and can be used to make high-strength, high-temperature-resistant, and waterproof materials. At present, the main researches on 3D printing technology of photosensitive materials are 3DSystem Company in the United States and Object Company in Israel. Israel's Object company has published four patents on photocurable 3D printing materials, and its photosensitive resin for jetting is used at around 70-75°C. The monomer ...

Claims

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Application Information

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IPC IPC(8): C08F283/12C08F220/18C08F220/14C08F2/38B33Y70/00
Inventor 钱永嘉杨伟张伟
Owner CHANGZHOU HUAKE POLYMERS
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