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Method for preparing methylphenyl hydrogen-containing silicone oil

A technology of methyl phenyl and polymethyl hydrogen cyclosiloxane is applied in the field of preparation of hydrogen-containing silicone oil to achieve the effects of convenient industrialization, simple operation and mild conditions

Inactive Publication Date: 2008-07-09
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This kind of hydrogen-containing silicone oil has not been sold on the market. Most of the methylphenyl hydrogen-containing silicone oils for LED packaging reported in foreign patents are hydrogen-containing silicone oils containing diphenylsiloxane chain links, while the LED packaging of the present invention contains The methylphenyl hydrogen-containing silicone oil of the methylphenylsiloxane chain has not been reported, and the hydrogen-containing silicone oil reported in domestic and foreign literature is basically formed by hydrolysis and polycondensation of hydrogen-containing chlorosilane and non-hydrogen-containing chlorosilane

Method used

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  • Method for preparing methylphenyl hydrogen-containing silicone oil
  • Method for preparing methylphenyl hydrogen-containing silicone oil
  • Method for preparing methylphenyl hydrogen-containing silicone oil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] in N 2 Add 63.8g of polymerized monomer to a 500mL dry three-neck flask under protection p Ph and 36.2gD 4 H , at 35℃~45℃ / -0.096MPa to remove the water in the polymerized monomer, and then add 2.6g of end-capping agent 1,1,3,3-tetramethyl-1,3-dihydrodisiloxane alkanes, 5.0 g catalyst (large pore size strongly acidic cation exchange resin), 100 mL toluene solvent, polymerize at 65° C. for 5 h, and recover the large pore size strong acid cation exchange resin by suction filtration. Atmospheric pressure through N 2 Evaporate most of the toluene under protection, then reduce the pressure to -0.096MPa, gradually raise the temperature to 205°C to remove the remaining solvent and low molecular weight compounds, cool to room temperature, add 1wt% powdered activated carbon of the total mass of the mixture and stir, then pump The powdered activated carbon was recovered by filtration, and the filtrate was colorless and transparent methylphenyl hydrogen-containing silicone oil...

Embodiment 2

[0033] Using the same method as in Example 1, with 37.1gD p Ph , 27.7gD 4 H , 35.2g D' q Ph 1.8g of 1,1,3,3-tetramethyl-1,3-dihydrodisiloxane as end-capping agent, 5.0g of large-pore strongly acidic cation exchange resin as catalyst, and 100mL of toluene as solvent , after the polymerization and post-treatment are completed, the refractive index n of the obtained methylphenyl hydrogen-containing silicone oil D 25 =1.4720, the rotational viscosity at 25°C is about 150mpa·s. through 1 H-NMR records Si-H mass percentage content 0.4%, Ph / Si (molar ratio) is 0.33, and GPC records number average molecular weight (Mn) and is 2.7 * 10 3 g.mol -1 , MWD is 1.69.

Embodiment 3

[0035] Adopt the method identical with embodiment 1, with 42.5gD p Ph , 15.1gD 4 H , 42.5g D' q Ph 2.5g of 1,1,3,3-tetramethyl-1,3-dihydrodisiloxane as the end-capping agent, 5.0g of large-pore strong acid cation exchange resin as the catalyst, and 100mL of toluene as the solvent , after the polymerization and post-treatment are completed, the refractive index n of the obtained methylphenyl hydrogen-containing silicone oil D 25 =1.4898, the rotational viscosity at 25°C is about 120mpa·s, after 1 H-NMR records Si-H mass percentage content 0.24%, Ph / Si (molar ratio) is 0.43, and GPC records number average molecular weight (Mn) and is 2.4 * 10 3 g.mol -1 , MWD is 2.27.

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Abstract

The invention discloses a process for preparing organosilicon oil which contains hydrogen, in particular to a process for preparing organosilicon oil which contains hydrogen and methyl-phenyl silica chain link. The invention utilizes dimethyl silicone cyclic siloxane(Dn), polymethyl hydrogen cyclic siloxane(DmH), hybrid ring body of methyl and phenyl (DpPh), hydrolysis hybrid ring body of methyl and phenyl (D'qPh) to be polymerization reaction monomer, the process comprises adding the polymerization reaction monomer and blocking agent into organic solvent under the protection of N2 gas, controlling the reaction temperature and the reaction time, reacting under the function of catalyst, distilling to remove dissolvent in ordinary pressure after reacting, decompressing to withdraw low-boiling residue to get target product, purifying the product with activated carbon, and then the degree of purity of the product is high. The invention has the advantages of low cost, moderate contiditon, simple technology, simple and convenient operation and no pollution, and raw material are easily obtained, and the invention is suitable for industrialization. Products which are prepared by the invention have an excellent effect in the process of sealing and packing of LED.

Description

technical field [0001] The invention relates to a method for preparing hydrogen-containing organic silicon oil, in particular to a method for preparing hydrogen-containing organic silicon oil containing methylphenylsiloxane chain members. technical background [0002] After decades of development, power light-emitting diodes (Light Emitting Diode, LED) are widely used in large-area graphic display full-color screens, status indications, sign lighting, signal displays, backlights for liquid crystal displays, automobile combination taillights and vehicle Internal lighting etc. LED has many unique advantages, as stated in "China Lighting" 2007 (1-2): 54-59, LED has energy saving, environmental protection, long life safety, low consumption, low heat, shockproof, waterproof, miniature, high brightness, easy to adjust Concentrated light and light beams and reduced maintenance and other advantages, using one or more of the above advantages or all of the advantages can develop many...

Claims

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Application Information

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IPC IPC(8): C08G77/12C08G77/08
Inventor 伍川蒋剑雄杨雄发邬继荣罗蒙贤
Owner HANGZHOU NORMAL UNIVERSITY
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