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Poly(diphenyl-dimethyl siloxane) with terminals sealed by alkyloxy groups, and preparation method thereof

A technology of polydiphenyldimethylsiloxane and polydimethylsiloxane, which is applied in the field of silicone materials, and can solve the problem of storage stability and heat resistance decline, affecting product transparency, and ring-opening reactivity Low-level problems, to achieve the effect of improving quality and transparency, improving storage stability, and easy operation

Active Publication Date: 2011-10-19
SHANDONG DONGYUE ORGANIC SILICON MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the large steric hindrance of octaphenylcyclotetrasiloxane, high melting point (about 200 ° C), and poor solubility in the ring body, resulting in low ring-opening reactivity, it is commonly used in the production of polydimethylsiloxane Acidic catalysts such as concentrated sulfuric acid, acid clay, ion exchange resins, lithium hydroxide, sodium hydroxide and silicon alkoxides of these alkalis usually cannot cause ring-opening polymerization.
CN101016446A reported the use of octaphenylcyclotetrasiloxane and dimethylsiloxane rings to prepare vinyl-terminated polydiphenyldimethylsiloxane under the catalysis of silicon alkoxide of potassium hydroxide, and then Preparation of addition-type silicone rubber for LED device packaging, but the polymerization temperature of this patented method is high and the time is long. Excessive silicon-based phosphate and neutralization product potassium phosphate will affect the transparency of the product and lead to product loss. Storage stability and heat resistance decline, and the product with a refractive index of 1.51 cannot be obtained according to the charging amount in Example 1 of this patent
In particular, under the catalysis of potassium silanolate and the action of accelerator, the process of preparing alkoxy-terminated polydiphenyldimethylsilane from octaphenylcyclotetrasiloxane according to the present invention has not been reported yet.

Method used

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  • Poly(diphenyl-dimethyl siloxane) with terminals sealed by alkyloxy groups, and preparation method thereof
  • Poly(diphenyl-dimethyl siloxane) with terminals sealed by alkyloxy groups, and preparation method thereof
  • Poly(diphenyl-dimethyl siloxane) with terminals sealed by alkyloxy groups, and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 2

[0056] Example 2, Preparation of 2# end-capping agent-polydimethylsiloxane whose end group contains two methoxy groups

[0057] Add the DMC of the methyltrimethoxysilane (KBM13) of 110g and 1000g in the reaction bottle, other raw material addition and implementation method are the same as embodiment 1, obtain colorless and transparent, colorless after polymerization, neutralization, filtration, take off. Dimethicone containing two methoxyl groups at the end of the odor. The viscosity of gained product is 22mPa s, and volatile matter content is 0.20%, and refractive index n D 20 is 1.4035.

Embodiment 3

[0058] Example 3, Preparation of Target Product-Methoxy-terminated Polydiphenyldimethylsiloxane

[0059] Add 65g of octaphenylcyclotetrasiloxane (D 4 Ph2 ) and the methoxy-terminated polydimethylsiloxane (hereinafter referred to as 1# end-capping agent) that the embodiment 1 of 300g obtains, then add silicon alkoxide potassium salt catalyst 0.2g and dimethyl sulfoxide (DMSO) 1.5 g. After sealing the reaction system, start stirring, and raise the temperature to 150°C. After about 10 minutes, the solid powder in the reaction bottle almost completely disappears, and the viscosity rises. After being constant for 4 hours, remove the heat source and start to cool down.

[0060] Add 0.3g of propionic acid to the reaction mixture cooled to 40°C, stir for 1 hour, transfer to a filter, pressurize to 0.15Mpa at room temperature, filter out solid impurities such as potassium acetate with ordinary filter paper, and obtain a colorless and transparent of the filtrate.

[0061] Transfer t...

Embodiment 4

[0062] Embodiment 4, as described in embodiment 3, the difference is:

[0063] Add 140g of octaphenylcyclotetrasiloxane (D 4 Ph2 ) and 300g of 1# end-capping agent, 0.3g of potassium silanolate catalyst and N,N-dimethylacetamide 2.5g. The temperature of the closed reaction system was raised to 150°C. After about 10 minutes, the solid powder in the reaction bottle almost completely disappeared, and the viscosity increased, and then the temperature was lowered after being constant for 5 hours.

[0064] The reaction mixture cooled to 40° C. was neutralized by adding 0.5 g of propionic acid, filtered to remove low molecules, and a colorless, transparent, odorless methoxy-terminated polydiphenyldimethylsiloxane product was obtained. The results are shown in Table 1.

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Abstract

The invention relates to a poly(diphenyl-dimethyl siloxane) with terminals sealed by alkyloxy groups, and a preparation method thereof. The preparation method comprises that octaphenylcyclotetrasiloxane and octamethylcyclotetrasiloxane as monomers for a polymerization reaction, low viscosity polydimethylsiloxane with terminals sealed by alkyloxy groups as a terminal sealing agent, and potassium silanolate as a catalyst are adopted; the monomers, the terminal sealing agent, the catalyst and accelerating agents are added into a reaction system; the reaction system is sealed up and then the mixture in the reaction system is stirred and heated to a temperature of 120 to 180 DEG C to undergo a polymerization reaction for 1 to 16 hours; and processes of neutralization, filtering and removal of low molecules on the reaction system are carried out. The preparation method has the advantages of high purity of raw materials, simple process, no need of a mass of organic solvents, and environmentally friendly characters. Products prepared by the preparation method has the advantages of high refractive index and good radiation resistance, high-low temperature resistance and climate resistance, and is especially suitable for base polymers of a dealcoholization type room temperature vulcanized silicone rubber, and surface treatment agents of filling materials such as white carbon black and the like utilized in various silicone rubber and other rubber processing.

Description

technical field [0001] The invention relates to a preparation method of linear polyorganosiloxane containing phenyl, belonging to the field of organosilicon materials. technical background [0002] The phenyl-containing polymethylphenylsiloxane can be considered as a product in which some of the methyl groups in the polydimethylsiloxane structure are replaced by phenyl groups. In addition to the common performance characteristics of polymethylsiloxane, It also has outstanding advantages such as excellent low temperature resistance, high temperature resistance, radiation resistance and high refractive index, and is widely used in the fields of electronic appliances, green energy, aerospace and life sciences. [0003] According to the structure of the siloxane chain where the phenyl group is located, it can usually be divided into polydiphenyldimethylsiloxane and polyphenylmethylsiloxane. The structural formula is as follows: [0004] [0005] Change the functional group o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/44
Inventor 胡生祥桑圣凯付佃亮
Owner SHANDONG DONGYUE ORGANIC SILICON MATERIAL
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