Method for preparing graphene photocurable resin nanomaterial, casting solution and casting method

A light-curing resin and nano-material technology, applied in the direction of additive processing, etc., can solve the problems of poor mechanical properties, insufficient toughness, high printing cost, etc., to improve tensile properties and bending properties, wide application range, and reduce volume shrinkage rate effect

Active Publication Date: 2020-05-05
恒信智能(天津)快速制造技术有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, most of the molding materials used in China rely on imports. Imported materials are expensive and printing costs are high. However, most of the domestically developed photosensitive resin materials have low hardness, insufficient toughness, and poor mechanical properties, which limit the application of light curing technology. Extend the application further

Method used

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  • Method for preparing graphene photocurable resin nanomaterial, casting solution and casting method
  • Method for preparing graphene photocurable resin nanomaterial, casting solution and casting method
  • Method for preparing graphene photocurable resin nanomaterial, casting solution and casting method

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Graphene photocurable resin nanomaterials include graphene oxide and photosensitive resin, and the preparation method of described graphene oxide is as follows:

[0028] (1) Preparation of graphene oxide

[0029] Add 3.0g of flake graphite and 1.5g of sodium nitrate into 69mL of concentrated sulfuric acid, oscillate ultrasonically for 20min in an ice bath, slowly add 18.0g of potassium permanganate, ultrasonicate for 5min below 20°C, and stir for 2h in a water bath at 35-40°C. Then transfer it to a constant temperature water bath at 90°C and stir for 30 minutes, cool to room temperature, add 400mL of ice water and stir to mix, then slowly add 3mL of 30% hydrogen peroxide and stir for 2h, filter, and successively wash with distilled water, 30% hydrochloric acid and ethanol Wash repeatedly, and centrifuge at 6000r / min for 10min to remove larger solids. Finally, the suspension is filtered with PTEE membrane, and the obtained solid is vacuum-dried at room temperature for 12...

Embodiment 2

[0033] Graphene photocurable resin nanomaterials include graphene oxide and photosensitive resin, and the preparation method of described graphene oxide is as follows:

[0034] (1) Preparation of graphene oxide

[0035] Add 3.0g flake graphite and 1g sodium nitrate into 68mL concentrated sulfuric acid, oscillate ultrasonically for 15min in an ice bath, slowly add 10g potassium permanganate, ultrasonicate for 8min below 20°C, stir for 2h in a water bath at 35-40°C, then Transfer it to a constant temperature water bath at 90°C and stir for 40 minutes, cool to room temperature, add 400 mL of ice water and stir to mix, then slowly add 3 mL of 30% hydrogen peroxide and stir for 2 hours, filter, and repeat with distilled water, 30% hydrochloric acid and ethanol in turn. Wash and centrifuge at a speed of 6000r / min for 10min to remove larger solids, and finally filter the suspension with a PTEE membrane, and dry the solid under vacuum at room temperature for 12h to obtain brown graphi...

Embodiment 3

[0039] Graphene photocurable resin nanomaterials include graphene oxide and photosensitive resin, and the preparation method of described graphene oxide is as follows:

[0040] (1) Preparation of graphene oxide

[0041]Add 3.0g of flake graphite and 3.0g of sodium nitrate into 75mL of concentrated sulfuric acid, oscillate ultrasonically for 15min in an ice bath, slowly add 40g of potassium permanganate, ultrasonicate for 8min below 20°C, and stir for 2h in a water bath at 35-40°C. Then transfer it to a constant temperature water bath at 90°C and stir for 40 minutes, cool to room temperature, add 800 mL of ice water and stir to mix, then slowly add 3 mL of 30% hydrogen peroxide and stir for 2 hours, filter, and repeat with distilled water, 30% hydrochloric acid and ethanol in sequence Wash and centrifuge at a speed of 6000r / min for 10min to remove larger solids. Finally, the suspension is filtered with a 0.25um PTEE membrane, and the resulting solid is vacuum-dried for 12h at r...

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Abstract

The invention discloses a method for preparing a graphene photocurable resin nanometer material. The method comprises the following steps: (1) preparing graphene oxide; (2) dropwise adding a mixing solution of acrylic acid, N,N-dimethylaniline and hydroxyanisole into epoxy resin with the temperature of 60 DEG C; heating, reacting at 100-110 DEG C until the acid value is between 4-5 mg.KOH / g, stopping heating, and obtaining a prepolymer; (3) adding the graphene oxide obtained from step (1) to the prepolymer obtained in the step (2), mixing, and then adding a trimethylolpropane triacrylate monomer and a photoinitiator, mixing and stirring in a dark room for 0.5 to 1 h, then carrying out ultrasonic mixing for 0.5 to 1h, removing bubbles in vacuum to obtain a tan pouring solution. The graphene oxide provided by the invention is added to increase the photo-curing rate of the nanometer material with a maximum curing rate of 96.6%.

Description

technical field [0001] The invention belongs to the technical field of materials for 3D printing, and in particular relates to the preparation and pouring method of graphene light-cured resin nanomaterials. Background technique [0002] 3D printing technology is a new type of manufacturing technology that emerged and developed in the late 1980s. Because its technology can process parts of any complexity, it can even make parts that are difficult to form by traditional technology, so it has developed rapidly. At present, 3D printing technology has been widely used in aerospace, automobile, mold, electronics, education and other fields. Photocuring molding is a typical process in 3D printing technology. The molding material is liquid photosensitive resin. The molding parts have the characteristics of good surface quality and high molding precision. At present, most of the molding materials used in China rely on imports. Imported materials are expensive and printing costs are ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F285/00C08F222/14C08F2/48C08K9/02C08K3/04B33Y70/10
CPCB33Y70/00C08F2/48C08F285/00C08K3/04C08K9/02C08K2201/011C08F222/14
Inventor 刘玉山孙淼陈少华
Owner 恒信智能(天津)快速制造技术有限公司
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