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Preparation method of polyurethane-modified organic silicon resin

A technology of polyurethane modification and silicone, applied in the direction of additive processing, etc., can solve the problems of poor performance, low mechanical strength, and large irritation

Active Publication Date: 2017-06-09
HANGZHOU LEYI NEW MATERIAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, UV-curable 3D printing polymers are mainly polyacrylates, epoxy resins, etc., due to matrix matching and formula design, etc., resulting in low curing efficiency, poor part performance, high irritation and high cost.
The molecular main chain of silicone resin is a skeleton composed of alternating Si-O-Si bonds, which combines the characteristics of organic polymers and inorganic compounds. This unique structure makes it have excellent high and low temperature resistance and excellent electrical insulation and chemical stability, but there are also disadvantages such as low mechanical strength and poor resistance to organic solvents.

Method used

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Examples

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preparation example Construction

[0018] The embodiment of the present invention discloses a method for preparing a polyurethane-modified silicone resin, comprising the following steps: under the action of a catalyst, performing a hydrolysis reaction on a silicone raw material with an epoxy group and an alkoxysilane in a first solvent, Obtaining a hydroxyl-terminated silicone resin prepolymer; reacting diisocyanate with polyether diol to obtain a polyurethane prepolymer; The reaction is carried out for 0.5-10 hours to obtain a polyurethane modified silicone resin; the polyurethane modified silicone resin is mixed with a photoinitiator, and the polyurethane modified silicone resin is obtained after vacuum defoaming.

[0019] As a preferred solution, the catalyst is preferably one or more of phosphoric acid, sodium dihydrogen phosphate, potassium dihydrogen phosphate, and acetic acid. The mass ratio of the catalyst to the alkoxysilane is preferably 1-8:100, more preferably 3-8:100.

[0020] As a preferred versi...

Embodiment 1

[0032](1) Add a mixture of 350g of water, 1200g of toluene and 95g of acetic acid into a 5L clean, nitrogen-protected three-necked flask, and then add 323g of γ-(2,3-epoxy Propoxy)propyltrimethoxysilane, a mixture of 450g dimethyldiethoxysilane, 68g methyltriethoxysilane and 41.6g ethyl orthosilicate, react at 60°C for 4h after the dropwise addition, and then wash with water To neutrality, the solvent was distilled off at 150°C / 20mmHg to obtain R / Si=1.20, epoxy group content 15%, 724g hydroxyl-terminated silicone resin (82.0% yield), and a viscosity of 7850cp.

[0033] (2) Add 177.6 g of TDI dropwise to a 1L three-necked flask containing 400 g of PEG-400 and 400 g of toluene at 40° C. for 0.5 h, continue the reaction for 4 h after the dropwise addition, and distill off the toluene under reduced pressure to obtain isocyanate-terminated Polyurethane prepolymer 577.6g.

[0034] (3) Take 500g of the silicone resin obtained in (1) and 50g of the polyurethane prepolymer obtained in...

Embodiment 2

[0037] (1) Add 650g of water, a mixture of 2400g of xylene and 1.25g of phosphoric acid to a 5L clean, nitrogen-protected three-necked flask, and then add 240g of 2-(3,4 -Epoxycyclohexyl)ethyltrimethoxysilane, a mixture of 680g dimethyldiethoxysilane and 120g methyltriethoxysilane, reacted at 50°C for 8h after the dropwise addition, and then washed with water until neutral , The solvent was distilled off at 150° C. / 20 mmHg to obtain R / Si=1.80, epoxy group content 5%, 780 g hydroxyl-terminated silicone resin (yield 75%), and a viscosity of 2350 cp.

[0038] (2) Add 16.99g of HDI dropwise to a 1L three-necked flask containing 500g of PEG-5000 and 500g of xylene at 60°C for 0.5h, continue the reaction for 5h after the addition is complete, and distill off the xylene under reduced pressure to obtain isocyanate terminal Based polyurethane prepolymer 517.0g.

[0039] (3) Take 500g of the silicone resin obtained in (1) and 10g of the polyurethane prepolymer obtained in (2), add them...

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Abstract

The invention provides a preparation method of an ultraviolet-curing polyurethane-modified organic silicon resin for 3D printing. The method comprises the following steps: carrying out hydrolysis reaction on epoxy-group-containing alkoxy silane to obtain an epoxy-group-containing hydroxyl-terminated silicone resin, carrying out reaction on the epoxy-group-containing hydroxyl-terminated silicone resin, diisocyanate and polyether dibasic alcohol to obtain a prepolymer, and reacting to obtain an epoxy-group-containing polyurethane-modified organic silicon resin; uniformly mixing the epoxy-group-containing polyurethane-modified organic silicon resin with an ultraviolet photosensitizer, and carrying out vacuum degassing to obtain the ultraviolet-curing polyurethane-modified organic silicon resin for 3D printing. After the polyurethane-modified organic silicon resin is printed by an ultraviolet 3D printer, the obtained product has low buckling deformation tendency, the Shore hardness is 35-65A, the tensile strength is 0.3-2.5 MPa, the water absorptivity is 1-4.5%, and the linear expansion coefficient is 0.4-1.4%.

Description

technical field [0001] The invention relates to the technical field of organic chemistry, in particular to a preparation method of polyurethane-modified silicone resin. Background technique [0002] 3D printing is a new type of three-dimensional model manufacturing technology that emerged and developed in the late 1980s. It is a technical integration of CAD / CAM, precision machinery, laser technology, and material science and engineering. It is a new technology with strong vitality. . 3D printing technology, also known as additive manufacturing technology, uses a computer to build a three-dimensional model of an object, and then relies on it as a direct molding technology, which can automatically and accurately manufacture objects of benevolent and complex shapes on a single device through program control. It solves many problems that are difficult to solve by traditional manufacturing methods, thereby shortening the manufacturing cycle of products and greatly improving prod...

Claims

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Application Information

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IPC IPC(8): C08G18/65C08G18/61C08G18/48C08G18/32C08G18/10C08G77/16C08L75/08B33Y70/00
Inventor 许兴泽
Owner HANGZHOU LEYI NEW MATERIAL TECH CO LTD
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