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A kind of quaternized fluorine-containing silicone oil and preparation method thereof

A silicone oil, quaternization technology, used in textiles, papermaking, fiber treatment, etc.

Active Publication Date: 2018-06-12
科凯精细化工(上海)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Based on this, it is necessary to provide a quaternized fluorine-containing silicone oil and a preparation method thereof for the problem of how to prepare a darkening finishing agent with a good darkening effect and a better fabric feel and comfort.

Method used

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  • A kind of quaternized fluorine-containing silicone oil and preparation method thereof
  • A kind of quaternized fluorine-containing silicone oil and preparation method thereof
  • A kind of quaternized fluorine-containing silicone oil and preparation method thereof

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preparation example Construction

[0027] Such as figure 1 Shown, the preparation method of the quaternized fluorine-containing silicone oil of an embodiment, comprises the steps:

[0028] S1: Add octamethylcyclotetrasiloxane, trifluoropropylmethylcyclotrisiloxane, ammonia-type coupling agent, end-capping agent and basic catalyst into a mixed solvent, and obtain it by solution polymerization and ring-opening polymerization Fluorinated amino silicone oil solution.

[0029] Specifically, add octamethylcyclotetrasiloxane, trifluoropropylmethylcyclotrisiloxane, ammonia type coupling agent, basic catalyst and mixed organic solvent into a four-necked flask, Under the stirring speed of rev / min, the above-mentioned raw materials are stirred evenly. Wherein, the four-necked flask is equipped with a stirrer, a reflux condenser and a thermometer.

[0030] After stirring evenly, heat up to a temperature of 60-85°C. At a stirring speed of 200-400 rpm and a temperature of 60-85°C, octamethylcyclotetrasiloxane, trifluoropr...

Embodiment 1

[0064] 20g octamethylcyclotetrasiloxane, 10g trifluoropropylmethylcyclotrisiloxane, 4g N-β-(aminoethyl)-γ-aminopropylmethyldimethoxysilane, 0.5g Add tetramethylammonium hydroxide and 75g of mixed solvent into a four-neck flask equipped with a stirrer and a reflux condensing tube quarter thermometer, stir and mix evenly at a speed of 300rmp / min, then raise the temperature to 70°C, react for 8 hours, and finally add 0.06 g end-blocking agent hexamethyldisiloxane, after reacting for 1.5 hours, a fluorine-containing amino silicone oil solution was obtained, wherein the mixed solvent used was a mixture of toluene and isopropanol, and its mass percentage was 20:80;

[0065] Add dimethylaminoethyl methacrylate to the fluorine-containing amino silicone oil solution obtained above, stir and mix evenly at a speed of 300rmp / min, then raise the temperature to 25°C, and react for 15 hours to obtain a modified fluorine-containing amino silicone oil solution, wherein, The molar ratio of prim...

Embodiment 2

[0070] 10g octamethylcyclotetrasiloxane, 20g trifluoropropylmethylcyclotrisiloxane, 4g N-β-(aminoethyl)-γ-aminopropylmethyldimethoxysilane, 0.5g Add tetramethylammonium hydroxide and 75g of mixed solvent into a four-neck flask equipped with a stirrer and a reflux condensing tube quarter thermometer, stir and mix evenly at a speed of 300rmp / min, then raise the temperature to 70°C, react for 8 hours, and finally add 0.06 g end-blocking agent hexamethyldisiloxane, after reacting for 1.5 hours, a fluorine-containing amino silicone oil solution was obtained, wherein the mixed solvent used was a mixture of toluene and isopropanol, and its mass percentage was 20:80;

[0071] Add dimethylaminoethyl methacrylate to the fluorine-containing amino silicone oil solution obtained above, stir and mix evenly at a speed of 300rmp / min, then raise the temperature to 25°C, and react for 15 hours to obtain a modified fluorine-containing amino silicone oil solution, wherein, The molar ratio of prim...

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Abstract

The invention relates to quaternized fluorine-containing organic silicone oil and a preparation method thereof. The preparation method comprises the following steps: (1) adding octamethylcyclotetrasiloxane, 1,3,5-tris(3,3,3-trifluoropropyl)methylcyclotrisiloxane, an ammonia type coupling agent and an alkali catalyst into a mixed solvent, using hexamethyldisiloxane as an end-capping agent, and conducting ring opening polymerization through solution polymerization reaction so as to obtain a fluorine-containing amino silicon oil solution; (2) adding dimethylaminoethyl methacrylate, and enabling Michael addition reaction so as to obtain the modified fluorine-containing amino silicon oil solution; (3) adding alkyl halide, enabling quaternization reaction, and conducting reduced pressure distillation to remove the mixed solvent so as to obtain the quaternized fluorine-containing organic silicone oil; (4) conducting water emulsification on the quaternized fluorine-containing organic silicone oil. According to the quaternized fluorine-containing organic silicone oil and the preparation method thereof, the prepared quaternized fluorine-containing organic silicone oil has an excellent color-deepening effect on textile, and meanwhile can also better keep style and hand feeling of the textile.

Description

technical field [0001] The invention relates to the technical field of textiles, in particular to a quaternized fluorine-containing silicone oil and a preparation method thereof. Background technique [0002] Amino silicone oil and various modified amino silicone oils are commonly used textile finishing auxiliaries. Due to the strong polarity of the amino functional group, it interacts with the hydroxyl and carboxyl groups on the fiber surface of the fabric, thereby forming a very firm directional adsorption with the fiber, making the amino silicone oil have a strong combination with the fiber. The chain segments substituted between the amino silicone oil and the fibers form chain rings, and since these chain rings can move freely, the friction coefficient between the fibers is reduced. Amino silicone oil can improve the feel of the fabric, making it soft, smooth, elastic, anti-wrinkle, antistatic, etc. Amino silicone oil can also be used as a darkening agent for dark synth...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F283/12C08F220/34C08F8/44C08G77/24D06M15/657
CPCC08F8/44C08F283/12C08F2800/10C08G77/24D06M15/657C08F220/343
Inventor 任一波周文张萍顾永欢
Owner 科凯精细化工(上海)有限公司