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Preparation method of ultra violet (UV) light curing-type polymethyl siloxane with methacrylate structure-contained side group

A technology of methacrylate and polymethylsiloxane, which is applied in the field of preparation of UV-curable methyl silicone oil materials, can solve problems such as expensive catalysts, low acrylate grafting efficiency, and easy crosslinking, and achieve Excellent low surface energy, excellent release effect, and good weather resistance

Inactive Publication Date: 2018-09-07
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The purpose of the present invention is to provide a method for preparing polymethylsiloxane with high grafting rate and low cost of methacrylic acid esterification with excellent performance, which solves the problem that the catalyst is expensive in the prior art and the reaction process is prone to crosslinking , low acrylate grafting efficiency, cumbersome and expensive preparation of photoinitiators in the curing process and other technical problems

Method used

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  • Preparation method of ultra violet (UV) light curing-type polymethyl siloxane with methacrylate structure-contained side group
  • Preparation method of ultra violet (UV) light curing-type polymethyl siloxane with methacrylate structure-contained side group
  • Preparation method of ultra violet (UV) light curing-type polymethyl siloxane with methacrylate structure-contained side group

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Experimental program
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Embodiment 1

[0029] Synthesis of polymethylsiloxane material (PSi-MA) with side group containing methacrylate structure.

[0030] Ethylene glycol methacrylate, asymmetric diene structure, self-made, controllable for Michael addition reaction, figure 1 It is the NMR spectrum of ethylene glycol methacrylate. The protons of the structure correspond to the NMR signal peaks one by one, and the integral ratio is consistent with the proton ratio, indicating that it is the target reactant.

[0031] Amino silicone oil, i.e. aminopolymethoxysiloxane, has a structure such as formula [1], a molecular weight of 8200, self-made, figure 2 It is the nuclear magnetic spectrum of amino silicone oil, and the structure corresponds to the nuclear magnetic proton peak one by one. Through integral calculation, m=100, n=5, and the molar content of aminomethylsiloxane is 4.8%.

[0032] Amino silicone oil (10.00 g, 0.00125 mol) and solvent tetrahydrofuran (100 mL) were added to a 250 mL three-neck flask equipped ...

Embodiment 2

[0034] Synthesis of polymethylsiloxane material (PSi-MA) with side group containing methacrylate structure.

[0035] The difference from Example 1 is that the molecular weight of amino silicone oil is 8200, m=90, n=10, and the molar content of aminomethylsiloxane is 10%.

[0036] Under the condition of not changing other conditions of Example 1, the weight parts of amino silicone oil and ethylene glycol acrylate methacrylate in the preparation process are respectively: 10 parts and 7 parts, the solvent consumption is constant, can use ethyl acetate, toluene, Xylene, methyl ethyl ketone, etc. replaced tetrahydrofuran, and the operation process remained unchanged. The nuclear magnetic spectrum and infrared characterization confirmed that PSi-MA was successfully prepared, and the grafting rate of methacrylate reached 95%. Designation PSi-MA02.

Embodiment 3

[0038] Synthesis of polymethylsiloxane material (PSi-MA) with side group containing methacrylate structure.

[0039] The difference from Example 1 is that the molecular weight of amino silicone oil is 8200, m=104, n=3, and the molar content of aminomethylsiloxane is 2.8%.

[0040] Under the condition of not changing other conditions of Example 1, the weight parts of amino silicone oil and ethylene glycol acrylate methacrylate in the preparation process are respectively: 10 parts and 2.5 parts, and the solvent consumption is constant, available ethyl acetate, toluene, Xylene, methyl ethyl ketone, etc. replaced tetrahydrofuran, and the operation process remained unchanged. The nuclear magnetic spectrum and infrared characterization confirmed that PSi-MA was successfully prepared, and the grafting rate of methacrylate reached 95%. Designation PSi-MA03.

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Abstract

The invention relates to a preparation method of ultra violet (UV) light curing-type polymethyl siloxane with methacrylate structure-contained side groups. Through a Michael addition reaction betweenasymmetric diene acrylic acid-ethylene glycol methacrylate and amino silicone oil, the difference in activity of double bonds of the asymmetric diene is large, the acrylic structure is preferentiallyadded with amino groups, the methacrylic acid structure is successfully linked to side chains of methyl silicone oil, and structurally controllable methyl silicone oil with methacrylate structure-contained side groups is obtained. The reaction grafting rate is high; the preparation method is highly effective, gentle and controllable; a conventional compound photoinitiator is selected and applied onto a substrate for UV curing, and the coated substrate is rapidly cured to form a film at room temperature; the preparation method is clean and pollution-free; the complicated production of a silicone oil-modified photoinitiator is avoided; and the prepared organic silicon has the advantages of high temperature resistance, good weather resistance, good electrical insulation, excellent release effect, low surface tension and the like, and is widely applied to the industries such as release coating, coatings, leather auxiliaries, packaging and the like.

Description

technical field [0001] The invention belongs to the field of polymer material science, in particular to a method for preparing an ultraviolet (UV) curable methyl silicone oil material. Background technique [0002] Polymethylsiloxane is methyl silicone oil, which has many excellent physical and chemical properties due to its unique chemical structure. The structure is mainly composed of silicon-oxygen bonds, which has excellent soft structure characteristics and high and low temperature resistance. And it can be used in a wide temperature range. In addition, compared with conventional polymers, the silicon-oxygen structure has excellent weather resistance, corrosion resistance, electrical insulation, ozone resistance, waterproof, flame retardancy, physiological inertia, etc. Performance, widely used in aerospace, daily materials, electrical and electronic, chemical machinery, medical and health, transportation and other national economy industries. [0003] At present, trad...

Claims

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Application Information

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IPC IPC(8): C08G77/388
CPCC08G77/388
Inventor 薛小强蒋必彪黄文艳杨宏军蒋其民孙佳悦
Owner CHANGZHOU UNIV
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