A kind of phenol-terminated polysiloxane and its preparation method and a kind of polysiloxane-polycarbonate copolymer

A technology of phenol-terminated polysiloxane and hydrosilane, which is applied in the field of polysiloxane preparation, can solve problems such as increased process complexity, easy yellowing of products, and no mention of platinum content, and achieves product performance without , low catalyst dosage, improved heat resistance and yellowing resistance

Active Publication Date: 2021-10-22
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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  • A kind of phenol-terminated polysiloxane and its preparation method and a kind of polysiloxane-polycarbonate copolymer
  • A kind of phenol-terminated polysiloxane and its preparation method and a kind of polysiloxane-polycarbonate copolymer
  • A kind of phenol-terminated polysiloxane and its preparation method and a kind of 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 a phenol-terminated polysiloxane, a preparation method thereof and a polysiloxane-polycarbonate copolymer. The method comprises the following steps: a) using a transition metal catalyst A to catalyze the reaction of tetramethyldisiloxane and a phenolic compound containing an allyl group to prepare a phenol-modified hydrosilane with a phenol group at one end and a silicon-hydrogen bond at the other end; b) using Rectification and separation under reduced pressure to obtain a phenol-modified hydrosilane with a purity of ≥99%; c) catalyzing B with a transition metal catalyst to perform hydrosilylation of the pure phenol-modified hydrosilane and vinyl-terminated polysiloxane A reaction is carried out to obtain a polysiloxane with a phenolic group at the end. The content of free allyl-containing phenolic compounds in the phenol-terminated polysiloxane is less than 100 ppm, the capping rate of phenol groups is more than 98%, and the residual metal platinum is less than or equal to 5 ppm. The phenol-terminated polysiloxane is used to prepare modified polycarbonate, and the obtained polysiloxane-polycarbonate copolymer has 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 Patents(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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