Fluorine-containing alkenyl polysiloxane, preparation method thereof and application

A technology of alkenyl polysiloxane and alkenyl siloxane, which can be used in coatings and other directions, can solve problems such as increasing environmental costs and potential safety hazards.

Active Publication Date: 2016-08-17
国科广化(南雄)新材料研究院有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this fluorine coating needs to be mixed with a solvent before it can be used, wh

Method used

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  • Fluorine-containing alkenyl polysiloxane, preparation method thereof and application
  • Fluorine-containing alkenyl polysiloxane, preparation method thereof and application
  • Fluorine-containing alkenyl polysiloxane, preparation method thereof and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0064] 100g tetravinyltetramethylcyclotetrasiloxane (344.66) (Aladdin), 278.64g heptadecafluoro-1-decanethiol (Aladdin) (480.18) and 0.5g 1,5-diazabicyclo [4.3.0] Non-5-ene (DBN) (Aladdin) catalyst was dissolved in 1000 mL of butanone, mixed evenly, and reacted at 20°C for 20 min. pass 1 The reaction was monitored by H-NMR. The unreacted monomer and solvent were removed by rotary evaporation under reduced pressure to obtain 360 g of light yellow oily liquid with a yield of 95.1%.

[0065] React 360g of the fluorine-containing segment compound obtained above, 300g of octamethylcyclotetrasiloxane (Aladdin), and 3.3g of trifluoromethanesulfonic acid at 0°C for 15 minutes, and then add 71g of hexamethyldisiloxane Alkane (162.38) (Aladdin) was capped for 0.5h. Finally, 2 g of 1,5-diazabicyclo[4.3.0]non-5-ene (DBN) (Aladdin) base was added for neutralization and filtration to obtain 673 g of oily liquid I with a yield of 92.1%.

Embodiment 2

[0067] 100g tetravinyltetramethylcyclotetrasiloxane (344.66) (Aladdin), 278.64g heptadecafluoro-1-decanethiol (Aladdin) (480.18) and 0.5g 1,5-diazabicyclo [4.3.0] Dissolve non-5-ene (DBN) catalyst in 1000ml of butanone, mix well, and react at 20°C for 20min. pass 1 The reaction was monitored by H-NMR. The unreacted monomer and solvent were removed by rotary evaporation under reduced pressure to obtain 360 g of light yellow oily liquid with a yield of 95.1%.

[0068] The above obtained 360g fluorine-containing segment compound, 300g octamethylcyclotetrasiloxane, and 3.3g trifluoromethanesulfonic acid were reacted at 0°C for 15min, and then 149g divinyltetramethylsiloxane ( 186.4) (Aladdin) was capped for 0.5h. Finally, 2 g of 1,5-diazabicyclo[4.3.0]non-5-ene (DBN) was added for neutralization and filtration to obtain 728 g of oily liquid II with a yield of 90.0%.

Embodiment 3

[0070] 100g of tetravinyltetramethylcyclotetrasiloxane (344.66), 278.64g of heptadecafluoromercaptan (480.18) and 0.5g of 1,5-diazabicyclo[4.3.0]non-5-ene (DBN ) catalyst was dissolved in 1000 mL of methyl ethyl ketone, mixed evenly, and reacted at 20° C. for 20 min. pass 1 The reaction was monitored by H-NMR. The unreacted monomer and solvent were removed by rotary evaporation under reduced pressure to obtain 360 g of light yellow oily liquid with a yield of 95.1%.

[0071]React 360g of the above-obtained fluorine-containing segment compound and 3.3g of trifluoromethanesulfonic acid at 0°C for 15min, then add 149g of divinyltetramethylsiloxane (186.4) (Aladdin) for end-capping treatment 0.5h. Finally, 2 g of 1,5-diazabicyclo[4.3.0]non-5-ene (DBN) (Aladdin) was added for neutralization and filtration to obtain 460 g of oily liquid III with a yield of 90.4%.

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Abstract

The invention belongs to the field of material chemical synthesis, and discloses fluorine-containing alkenyl polysiloxane, a preparation method thereof and an application. The preparation method for the fluorine-containing alkenyl polysiloxane mainly comprises the following steps: (1) under the action of a solvent and a catalyst, enabling alkenyl siloxane units M1, D1 and T1 to react with a nucleophilic reagent of a fluorine-containing chain segment R3X, and purifying the obtained reaction liquor after the reaction is ended, thereby obtaining fluorine-containing alkenyl polysiloxane M, D and T; and (2) enabling at least one of D and T and at least one of D1, T1 and Q to generate hydrolytic condensation reaction under the action of the catalyst, adding M or M1 to generate end capping reaction after the reaction is ended, and purifying the reaction product to obtain the fluorine-containing alkenyl polysiloxane with a line-type or a body-type structure. The fluorine-containing alkenyl polysiloxane is added, so that a solvent-free organic polysiloxane composite forms a surface with lower surface energy, and therefore, a fluoride-containing siloxane anti-adhesion coating with lower release force is obtained.

Description

technical field [0001] The invention belongs to the field of chemical synthesis of materials, in particular to a fluorine-containing alkenyl polysiloxane and its preparation method and application. Background technique [0002] With the continuous acceleration of the pace of social development, silicone release materials have experienced the development trend from condensation solvent type to solvent-free addition type and then to emulsion type release agent. At present, the release materials used in industrial production are also developing in the direction of green environmental protection, fast curing at high temperature, low and uniform coating amount. Chinese patent publication CN1872927A relates to a high-viscosity polysiloxane composition, which is mainly composed of high-viscosity alkenyl polyorganosiloxane, crosslinking agent, catalyst, solvent and inhibitor. Chinese patent publication CN101531868A relates to the preparation of a high-solid content silicone anti-st...

Claims

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Application Information

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IPC IPC(8): C08G77/28C08G77/24C08G77/20C09D183/08C09D183/05
CPCC08G77/20C08G77/24C08G77/28C08L2205/02C08L2205/025C08L2205/03C08L2205/035C09D183/08C08L83/08C08L83/04
Inventor 胡继文杨公华张培魏彦龙邹海良涂园园林树东陈又军姚文英马红强
Owner 国科广化(南雄)新材料研究院有限公司
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