Preparation method of low-polymerization degree hydroxyl-terminated fluorosilicone oil

A technology of hydroxyl-blocked and fluoro-terminated silicone oil, applied in the direction of silicone organic compounds, can solve the problem of zero, and achieve the effects of simple equipment and process, low cyclosiloxane content, and mild reaction conditions

Active Publication Date: 2013-01-30
杭州科佳新材料股份有限公司
View PDF4 Cites 7 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to solve the problem that complex mixtures of linear polymers and cyclic siloxanes are often obtained in the process of preparing hydroxyl-terminated fluorosilicone oil with a low degree of polymerization, the present invention provides a method for preparing hydroxyl

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation method of low-polymerization degree hydroxyl-terminated fluorosilicone oil

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0023] Example 1

[0024] In a 3 L three-necked flask equipped with a thermometer, mechanical stirring and constant pressure dropping funnel, 800 mL of deionized water, 202 g of poly(4-vinylpyridine) (1.92 mol N) and 400 mL of ether were added at room temperature. Reduce the temperature in the reaction flask to 0 o C, then add 200 mL 3,3,3-trifluoropropylmethyldichlorosilane (2.4 mol Cl) dropwise to the three-necked flask at a constant speed through a constant pressure dropping funnel with sufficient stirring. After the addition is complete, continue stirring for 10 min, stop the reaction, and transfer the reaction mixture to a separatory funnel. Let stand, separate into layers, discard the lower aqueous solution, then wash the organic phase with deionized water to neutrality, collect the organic phase and pass it over anhydrous Na 2 SO 4 Dry overnight, and finally at less than 40 o The solvent was distilled off under reduced pressure under C to obtain a colorless and transparent...

Example Embodiment

[0025] Example 2

[0026] In a 3 L three-necked flask equipped with a thermometer, mechanical stirring and a constant pressure dropping funnel, 1200 mL of deionized water, 253 g (2.4 mol N) of poly(2-vinylpyridine) and 600 ethyl acetate were added at room temperature. mL, reduce the temperature in the reaction flask to –5 o C, then add 400 mL of 3,3,3-trifluoropropylmethyldichlorosilane (2.4 mol Cl) ethyl acetate solution with a volume concentration of 50% through a constant pressure dropping funnel with sufficient stirring Into a three-necked flask. After the addition is complete, continue stirring for 10 min, stop the reaction, and transfer the reaction mixture to a separatory funnel. Let stand, separate into layers, discard the lower aqueous solution, then wash the organic phase to neutral with deionized water, collect the organic phase at 50 o Bubbling with nitrogen gas at C and distilling under reduced pressure to remove residual moisture and organic solvents, a colorless a...

Example Embodiment

[0027] Example 3

[0028] In a 3 L three-necked flask equipped with a thermometer, mechanical stirring and a constant pressure dropping funnel, 1000 mL of deionized water and poly( N -Vinyl imidazole) 271 g (2.88 mol N) and 1000 mL ether, reduce the temperature in the reaction flask to 0 o C, then add 200 mL 3,3,3-trifluoropropylmethyldichlorosilane (2.4 mol Cl) dropwise to the three-necked flask at a constant speed through a constant pressure dropping funnel with sufficient stirring. After the addition is complete, continue stirring for 10 min, stop the reaction, and transfer the reaction mixture to a separatory funnel. Let stand, separate into layers, discard the lower aqueous solution, then wash the organic phase to neutral with deionized water, collect the organic phase at 50 o Bubbling with nitrogen gas at C and distilling under reduced pressure to remove residual moisture and organic solvents, a colorless and transparent hydroxyl-terminated fluorosilicone oil with a yield of...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention relates to the technical field of an organic silicon industry and provides a preparation method of low-polymerization degree hydroxyl-terminated fluorosilicone oil. The preparation method solves the problem that the existing preparation technology of low-polymerization degree hydroxyl-terminated fluorosilicone oil produces a complex mixture of a linear polymer and a cyclic siloxane. The low-polymerization degree hydroxyl-terminated fluorosilicone oil is a hydroxyl-terminated 3,3,3-trifluoropropylmethylsiloxane oligomer. The low-polymerization degree hydroxyl-terminated fluorosilicone oil obtained by the preparation method has an average polymerization degree of 1 to 5, high hydroxyl content, high purity and very low cyclic siloxane content, wherein the lowest cyclic siloxane content is 0.

Description

technical field [0001] The invention relates to the technical field of organosilicon industry, in particular to a preparation method of hydroxyl-terminated fluorosilicone oil with a low degree of polymerization. Background technique [0002] Fluorocarbon-based polysiloxane (fluorosilicone oil for short), due to the introduction of fluorine atoms in the molecular structure, compared with dimethyl silicone oil, the lubricating performance, oil resistance, and solvent resistance of fluorosilicone oil are particularly outstanding. , mineral oil lubricating oil, synthetic lubricating oil and most organic solvents all have anti-dissolution properties. Lubricants, defoamers, release agents and waterproof and antifouling finishing agents for fabrics and leathers prepared from them have been used in It has been widely used in aircraft, automobile, machinery, chemical industry, light industry, textile and other industrial fields. Among them, the hydroxyl-terminated fluorosilicone oil...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
IPC IPC(8): C07F7/08
Inventor 邬继荣胡应乾来国桥王华兰张国栋蒋剑雄
Owner 杭州科佳新材料股份有限公司
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap