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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
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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-terminated fluorosilicone oil with a low degree of polymerization. The low-polymerization-degree hydroxyl-terminated fluorosilicone oil prepared by the invention has high hydroxyl content and high purity, and the content of siloxane rings in the product is extremely low or even zero

Method used

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

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Embodiment 1

[0024] In a 3 L three-neck flask equipped with a thermometer, mechanical stirring and a constant pressure dropping funnel, 800 mL of deionized water, 202 g of poly(4-vinylpyridine) (1.92 mol N) and 400 mL of diethyl ether were sequentially added at room temperature, Lower the temperature in the reaction flask to 0 o C. Then, under full stirring, 200 mL of 3,3,3-trifluoropropylmethyldichlorosilane (2.4 mol Cl) was added dropwise to the three-neck flask through the constant pressure dropping funnel at a constant speed. After the dropwise addition was completed, stirring was continued for 10 min to stop the reaction, and the reaction mixture was transferred to a separatory funnel. Stand still, separate layers, let go of the lower aqueous solution, then wash the organic phase with deionized water until neutral, collect the organic phase and wash it with anhydrous Na 2 SO 4 Dry overnight and finally at below 40 o Under the condition of C, the solvent was distilled off under redu...

Embodiment 2

[0026] In a 3 L three-neck flask equipped with a thermometer, mechanical stirring and a constant pressure dropping funnel, 1200 mL of deionized water, 253 g of poly(2-vinylpyridine) (2.4 mol N) and 600 mL of ethyl acetate were added successively at room temperature. mL, reduce the temperature in the reaction flask to –5 o C, then under full stirring, 400 mL of 3,3,3-trifluoropropylmethyldichlorosilane (2.4 mol Cl) ethyl acetate solution with a volume concentration of 50% was added dropwise at a constant speed through a constant pressure dropping funnel into a three-neck flask. After the dropwise addition was completed, stirring was continued for 10 min to stop the reaction, and the reaction mixture was transferred to a separatory funnel. Let stand, separate layers, let off the aqueous solution of the lower layer, then use deionized water to wash the organic phase to neutrality, collect the organic phase at 50 o C under nitrogen bubbles, vacuum distillation to remove residual...

Embodiment 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, poly( N -vinylimidazole) 271 g (2.88 mol N) and ether 1000 mL, the temperature in the reaction flask was reduced to 0 o C. Then, under full stirring, 200 mL of 3,3,3-trifluoropropylmethyldichlorosilane (2.4 mol Cl) was added dropwise to the three-neck flask through the constant pressure dropping funnel at a constant speed. After the dropwise addition was completed, stirring was continued for 10 min to stop the reaction, and the reaction mixture was transferred to a separatory funnel. Let stand, separate layers, let off the aqueous solution of the lower layer, then use deionized water to wash the organic phase to neutrality, collect the organic phase at 50 o C under nitrogen bubbles, vacuum distillation to remove residual water and organic solvents, to obtain colorless and transparent hydroxyl-terminated fluorosilicone oil, yie...

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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

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Application Information

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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
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