Method for preparing methyl phenyl hydrogen-containing silicone oil by rare earth super acid catalysis

A technology of methylphenyl cyclosiloxane and methylphenyl, which is applied in the field of rare earth superacid catalyzed preparation of methylphenyl hydrogen-containing silicone oil, can solve problems such as pollution and complicated preparation process, and achieve simple process and labor-intensive Low, easy-to-operate effect

Inactive Publication Date: 2010-10-06
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] Aiming at the problem that the preparation process of LED packaging materials in the prior art is complicated and there is pollution at the same time, the present invention provides a method of using rare earth superacids to catalyze the ring-opening polymerization of cyclosiloxane to prepare highly clear and transparent hydrogen-containing silicone oil, which is used as an LED Crosslinking agent for encapsulation materials

Method used

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  • Method for preparing methyl phenyl hydrogen-containing silicone oil by rare earth super acid catalysis
  • Method for preparing methyl phenyl hydrogen-containing silicone oil by rare earth super acid catalysis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] in N 2 Add methylphenylcyclosiloxane monomer D to a 100mL dry three-neck flask under protection n Me,Ph (Mixtures of n=3, 4, 5 or 6 prepared by myself in any proportion) (34.50g, 0.2537mol of methylphenylsiloxane chain), D4 (27.10g, dimethylsiloxane chain section 0.3662mol) and D 4 H (0.40g, 0.0067mol of methyl hydrogen siloxane chain unit), remove the water in polysiloxane monomer at 35℃~45℃ / -0.096MPa, and then add end-capping agent 1,1,3, 3-Tetramethyl-1,3-dihydrodisiloxane (0.67g, 0.005mol), rare earth solid superacid TiO 2 / SO 4 2- / Nd 3+ (3.1g, 5% of the total monomer mass), at N 2 Under protection, polymerize at 100° C. for 5 h, and recover the catalyst by suction filtration. Reduce the pressure to -0.096MPa, gradually raise the temperature to 205°C to remove low-molecular compounds, stop heating when there is no fraction within 5 minutes, and cool to room temperature to obtain the product, whose refractive index is n D 25 =1.4950, dynamic viscosity 300...

Embodiment 2

[0029] in N 2 Add methylphenylcyclosiloxane monomer D to a 100mL dry three-neck flask under protection n Me,Ph (Mixtures of n=3, 4, 5 or 6 prepared by myself in any proportion) (40.55g, 0.2982mol of methylphenylsiloxane chain), D4 (21.50g, dimethylsiloxane chain section 0.2905mol) and D 4 H (0.4g, 0.0067mol of methyl hydrogen siloxane chain unit), remove the water in polysiloxane monomer at 35℃~45℃ / -0.096MPa, and then add end-capping agent 1,1,3, 3-Tetramethyl-1,3-dihydrodisiloxane (0.67g, 0.005mol), rare earth solid superacid TiO 2 / SO 4 2- / Nd 3+ (3.1g, 5% of the total monomer mass), at N 2 Under protection, polymerize at 100° C. for 5 hours, and recover the rare earth solid superacid catalyst by suction filtration. Reduce the pressure to -0.096MPa, gradually raise the temperature to 205°C to remove low-molecular compounds, stop heating when there is no fraction within 5 minutes, and cool to room temperature to obtain the product, whose refractive index is n D 25 ...

Embodiment 3

[0031] in N 2 Add methylphenylcyclosiloxane monomer D to a 100mL dry three-neck flask under protection n Me,Ph (Mixtures of n=3, 4, 5 or 6 prepared by myself in any proportion) (46.35g, 0.3408mol of methylphenylsiloxane chain), D4 (15.65g, dimethylsiloxane chain section 0.2115mol) and D 4 H (0.4g, 0.0067mol), remove the water in polysiloxane monomer at 35℃~45℃ / -0.096MPa, then add end-capping agent 1,1,3,3-tetramethyl-1 ,3-Dihydrodisiloxane (0.67g, 0.005mol), rare earth solid superacid TiO 2 / SO 4 2- / Nd 3+ (3.1g, 5% of the total monomer mass), at N 2 Under protection, polymerize at 100° C. for 5 hours, and recover the rare earth solid superacid catalyst by suction filtration. Reduce the pressure to -0.096MPa, gradually raise the temperature to 205°C to remove low-molecular compounds, stop heating when there is no fraction within 5 minutes, and cool to room temperature to obtain the product, whose refractive index is n D 25 =1.5120, dynamic viscosity 400mPa??S ， thr...

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Abstract

The invention discloses a method for preparing methyl phenyl hydrogen-containing silicone oil by rare earth super acid catalysis, which comprises the following steps of: taking methyl phenyl cyclosiloxane (DnMe, Ph, wherein n=3, 4, 5, 6), dimethyl cyclosiloxane (Dn, wherein n=3, 4, 5, 6), and methylhydrocyclosiloxane (DnH, wherein n=3, 4, 5, 6) as monomers; adding a blocking agent; and selecting rare earth super acids, controlling the reaction temperature, performing polymerization for a certain period under the protection of N2 gas, gradually raising the temperature to 205 DEG C under -0.9 MPa, and extracting low-boiling substances under reduced pressure to obtain the target product. The method has the advantages that: the catalyst can be separated only by filtering without washing neutralization, and the method has low labor intensity, simple process, simple and convenient operation and no pollution, and is convenient for industrialization. The product prepared by the method has good effects in the LED packaging process.

Description

technical field [0001] The invention relates to the technical field of preparing organosilicon polymer compounds, in particular to a method for preparing methylphenyl hydrogen-containing silicone oil catalyzed by rare earth superacids. technical background [0002] Ultra-high-brightness light-emitting diodes (Light Emitting Diode, LED) consume only 1 / 10 of the power of traditional light sources, do not use mercury that seriously pollutes the environment, are small in size and long in life, and have been used in decorative lighting, automotive lighting, and traffic lights. It is expected to become the fourth-generation light source after incandescent lamps, fluorescent lamps, and high-intensity gas discharge lamps. [0003] LED packaging materials need to have excellent light efficiency, high refractive index ( n D 25 >1.50,) and high light transmittance (that is, in the range of visible light (400~800nm), the light transmittance is greater than 98%, 10mm). Bisphenol ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/12C08G77/08C08L83/05C09J183/05C09K3/10
Inventor 来国桥杨雄发蒋剑雄邵倩伍川
Owner HANGZHOU NORMAL UNIVERSITY
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