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Phenol-terminated polysiloxane, preparation method thereof, and polysiloxane-polycarbonate copolymer

A technology of phenol-terminated polysiloxane and hydrogen silane is applied in the field of preparation of polysiloxane, which can solve the problems of easy yellowing of products, increase process complexity, and no mention of platinum content, and achieve free phenol content. Reduced, good blending and dispersibility, low dosage

Active Publication Date: 2020-02-11
WANHUA CHEM GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this patent increases the complexity of the process, and does not mention how to reduce the platinum content in polysiloxane with phenolic terminal groups, which makes the product prone to yellowing

Method used

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  • Phenol-terminated polysiloxane, preparation method thereof, and polysiloxane-polycarbonate copolymer
  • Phenol-terminated polysiloxane, preparation method thereof, and polysiloxane-polycarbonate copolymer
  • Phenol-terminated polysiloxane, preparation method thereof, and polysiloxane-polycarbonate copolymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] Embodiment 1 Eugenol modified hydrosilane synthesis

[0055] In a 1L three-necked flask, add 163 parts of eugenol (parts by mass, the same below) and Castel (tetramethyldivinyldisiloxane-platinum complex) catalyst (calculated as eugenol and tetramethyl 1 ppm of the total amount of disiloxane), the temperature was raised to 150° C., 134 parts of tetramethyldisiloxane was slowly added dropwise, and the reaction was continued for 1 h after the dropwise addition was completed. After the reaction is completed, use vacuum distillation, 30 theoretical plates, and a reflux ratio of 1:1 to extract the fraction at 163-169 ° C under a pressure of 50 Pa to obtain eugenol-modified hydrosilane (IIa) with a purity of 99.2%.

Embodiment 2

[0056] Example 2 Synthesis of 4-allylphenol modified hydrosilane

[0057] In a 1L three-necked flask, add 134 parts of 4-allylphenol (parts by mass, the same below) and chloroplatinic acid catalyst (calculated as 20ppm of the total amount of 4-allylphenol and tetramethyldisiloxane by platinum) , at 20°C, 670 parts of tetramethyldisiloxane was slowly added dropwise, and the reaction was continued for 10 h after the dropwise addition was completed. After the reaction is completed, use vacuum distillation, 20 theoretical plates, and a reflux ratio of 1:5 to extract the fraction at 156-162°C under a pressure of 60Pa to obtain 4-allylphenol-modified hydrosilane (IIb), with a purity of 99.5%.

Embodiment 3

[0058] Example 3 Synthesis of eugenol-modified hydrosilane

[0059] In a 1L three-necked flask, add 164 parts of eugenol (parts by mass, the same below) and Castel (tetramethyldivinyldisiloxane-platinum complex) catalyst (calculated as eugenol and tetramethyl 5ppm of the total amount of disiloxane), the temperature was raised to 70°C, and 402 parts of tetramethyldisiloxane was slowly added dropwise, and the reaction was continued for 4 hours after the dropwise addition was completed. After the reaction was completed, use vacuum distillation, 25 theoretical plates, reflux ratio 1:3, extract the fraction at 185-191°C under the pressure of 100Pa to obtain eugenol-modified hydrosilane (IIc) with a purity of 99.3%.

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Abstract

The invention discloses phenol-terminated polysiloxane, a preparation method thereof, and a polysiloxane-polycarbonate copolymer. The method includes the following steps: a) catalyzing a reaction of tetramethyldisiloxane and an allyl-containing phenolic compound by using a transition metal catalyst A to prepare phenol-modified hydrogen-containing silane having a phenol group at one end and a silicon-hydrogen bond at one end; b) performing separation by using reduced-pressure rectification to obtain phenol-modified hydrogen-containing silane with purity of >=99%; and c) catalyzing B by using atransition metal catalyst, performing a hydrosilylation reaction on the pure phenol-modified hydrogen-containing silane and polysiloxane with a vinyl end group to obtain the polysiloxane containing aphenol group at the end group. The content of the free allyl-containing phenol compound in the phenol-terminated polysiloxane is 100 ppm or less, the phenol group capping rate is 98% or more, and theresidual metal platinum content is <= 5 ppm. The phenol-terminated polysiloxane is used for preparing the modified polycarbonate, and the obtained polysiloxane-polycarbonate copolymer has a high polysiloxane content, and excellent heat resistance and yellowing resistance.

Description

technical field [0001] The invention relates to a preparation method of polysiloxane, in particular to a polysiloxane used for modifying polycarbonate and a preparation method thereof, and also relates to modified polycarbonate. Background technique [0002] Polycarbonate has good mechanical properties such as transparency and impact resistance, so it is widely used in automobiles, electronics, electrical appliances and other fields. In order to improve the flame retardancy, impact resistance and other properties of polycarbonate, it has been reported in the literature that polysiloxane is used as a comonomer to prepare polysiloxane-polycarbonate copolymers. [0003] The method of polysiloxane modified polycarbonate reported in the literature is divided into three steps at present: 1, the synthesis terminal group is the polysiloxane of silicon-hydrogen bond; 3. The polysiloxane whose terminal group is phenolic group is used as a comonomer to participate in the synthesis of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/38C08G77/20C08G77/448
CPCC08G77/20C08G77/38C08G77/448
Inventor 张聪颖曹骏高源杨继朋刘盼盼邱化敏周亚文王玉彬
Owner WANHUA CHEM GRP CO LTD
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