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Method for anhydrous synthesis of organosiloxane resin and product thereof, and application of product

A technology for organosiloxane and dimethyldisiloxane, which is applied in the field of anhydrous synthesis of organosiloxane resins, can solve the problems of poor environmental protection performance, poor process reproducibility, low yield and the like, and avoid gelation. The effect of sizing and narrowing the molecular weight distribution

Active Publication Date: 2017-10-03
GUANGDONG BIOMAX SIANDF NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In summary, the synthesis of silicone resins mainly revolves around the method of co-hydrolysis polycondensation: adding water to provide hydroxyl groups and then further condensing them into resins. This method generally has complex processes, long production cycles, poor environmental performance, easy gelation, and high yield. Low efficiency, poor process reproducibility, high energy consumption, etc.
More importantly, it is not possible to prepare silicone resins with narrow molecular weight distributions and related structures

Method used

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  • Method for anhydrous synthesis of organosiloxane resin and product thereof, and application of product
  • Method for anhydrous synthesis of organosiloxane resin and product thereof, and application of product
  • Method for anhydrous synthesis of organosiloxane resin and product thereof, and application of product

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preparation example Construction

[0059] The invention provides the synthetic method of this product, comprising:

[0060]1) Take alkoxysilane, capping agent and acidic compound according to the molar ratio of 1:(0-2):(2-10), mix and stir evenly, and stir at 40-100°C for 0.3-20h;

[0061] Alkoxysilanes are trifunctional and / or tetrafunctional alkoxyorganosilanes, and acidic compounds include organic carboxylic acids and acidic catalysts;

[0062] 2) cooling, adjusting the pH to 1-12, standing for stratification, and removing the water phase;

[0063] 3) After drying and filtering, distill under reduced pressure at 20-180°C to obtain a silicone resin.

[0064] This method prepares higher quality silicone resin by avoiding the use of water in the synthesis process. Compared with the cohydrolysis polycondensation method, the silicone resin obtained by this method has a narrower molecular weight distribution and more controllable molecular weight. This method can be applied to MT Synthesis of resins, MQ and MTQ ...

Embodiment 1

[0068] Embodiment 1 provides the synthesis method of methacryloxypropyl MT silicone resin, the specific operations are as follows: octyltriethoxysilane (138.25g, 0.5mol), hexamethyldisiloxane (4.06g, 0.025mol), glacial acetic acid (99.08g, 1.65mol) and 98wt% sulfuric acid (1.4g) were added into a round bottom flask, stirred evenly, and heated to 78°C for 4 hours under reflux. After cooling to room temperature, the resulting reaction mixture was neutralized to pH=7 with aqueous sodium carbonate solution (15 wt%, 198.29 g). The organic phase was separated by decantation, and the organic solvent was removed under reduced pressure at 80 °C to obtain a viscous liquid resin. GPC measurement showed that Mn=1554, Mw=1829 and PDI=1.1770 of the resin.

Embodiment 2

[0070] Embodiment 2 provides the synthetic method of methacryloxypropyl MTQ silicone resin, and concrete operation is as follows: Tetraethoxysilane (10.42g, 0.05mol), hexamethyldisiloxane (4.06g, 0.025mol ), 3-methacryloxypropyltrimethoxysilane (3.72g, 0.015mol), glacial acetic acid (14.70g, 0.245mol) and 98wt% sulfuric acid (0.18g, 110ul) were stirred in a round bottom flask, Heat to 50°C for 4 hours. After cooling to room temperature, the resulting mixture was neutralized to pH=7 with aqueous sodium carbonate solution (20 wt%, 3.42 g). The organic phase was separated by decantation, and the organic solvent was removed under reduced pressure at 60 °C to obtain a viscous liquid resin. The product has Mn=1462, Mw=2328, PDI=1.59.

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Abstract

The invention discloses an organosiloxane resin product prepared through anhydrous synthesis. The product is prepared by subjecting alkoxy silane, an end-capping reagent and an acidic compound in a mol ratio of 1: (0-2): (2-10) to a reaction, wherein the alkoxy silane is trifunctional and / or tetrafunctional alkoxy silane, and the acidic compound comprises organic carboxylic acid and an acidic catalyst. The organosiloxane resin provided by the invention has high regularity, narrower molecular weight distribution and PDI of less than 1.8. The invention also provides a preparation method for the organosiloxane resin. According to the method, an anhydrous one-step synthesis process is employed; and changes of the molecular weight parameters of polymers can be induced in a predicted way by controlling a pH value during quenching and the temperature of pressure-reduced distillation. The invention also provides application of the product. Since the organosiloxane resin product has good regularity, the organosiloxane resin product has good application prospects in silicone rubber, adhesives, lubricants, release agents and personal care products.

Description

technical field [0001] The invention relates to a siloxane and its organosiloxane resin, in particular to a method, product and application for anhydrous synthesis of an organosiloxane resin. Background technique [0002] At present, silicone resin is an important commercial material, which is widely used in coatings, electronics, construction, industrial chemicals, personal care, medical devices, etc. due to its good properties such as high temperature resistance, hydrophobicity, and insulation Many areas [1] . Its ability to form a network can be distinguished by different silane units. For example, the MQ type of silicone resin studied in this paper is composed of monofunctional units (R 3 SiO 1 / 2 , called M units) and tetrafunctional units (SiO 4 / 2 , known as Q units); MT-type silicone resins consist of monofunctional units (R 3 SiO 1 / 2 , called M units) and trifunctional units (RSiO 3 / 2 , referred to as T unit). [0003] At present, the preparation of MQ silicon...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/14C08G77/16C08G77/06
CPCC08G77/06C08G77/14C08G77/16C08G77/70
Inventor 伍锦枢陈贤惠黄振宏陈扬迈克·亚当·布鲁克
Owner GUANGDONG BIOMAX SIANDF NEW MATERIAL CO LTD
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