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Fluoride-containing silicone oil defoamer and preparation method thereof

A technology of fluorine-containing silicone oil and defoamer, which is applied in the direction of foam dispersion/prevention to achieve the effects of suppressing foam, simple process flow, increasing high temperature resistance and chemical stability

Active Publication Date: 2015-04-01
ZHEJIANG JUHUA HANZHENG NEW MATERIAL +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the commonly used defoamer in industry is silicone defoamer. However, silicone has a certain solubility in the oil phase, and it is difficult to meet the needs of industrial production by using silicone alone as a defoamer.

Method used

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  • Fluoride-containing silicone oil defoamer and preparation method thereof
  • Fluoride-containing silicone oil defoamer and preparation method thereof
  • Fluoride-containing silicone oil defoamer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] (1) Put 60g of hexafluoropropylene dimer and 23.2g of potassium fluoride into a three-necked flask with a reflux condensing device, then add 30mL of anhydrous DMF, heat to 60°C under stirring, and then add 24g of allyl bromide with The dropping funnel was added dropwise into the reaction bottle, and the dropwise addition was completed in 1.0 hour. After continuing to react at constant temperature for 26 hours, cool to room temperature, add 300 mL of water to the reaction solution, extract three times with 300 mL of ether, combine the organic phases, and separate the organic phases by rectification to obtain 50.0 g of fluorine-containing olefins with a yield of 68%.

[0042] (2) Add 120 g of fluorine-containing olefin into a 250 mL autoclave, and then add Karstede catalyst into the autoclave. The amount of Karstede catalyst used is 30 ppm of the mass of methyldichlorosilane. Seal the reaction kettle, start stirring and heating, so that the temperature of the reaction ket...

Embodiment 2

[0046] (1) Put 60g of hexafluoropropylene dimer and 23.2g of potassium fluoride into a three-necked flask with a reflux condensing device, then add 30mL of anhydrous DMF, heat to 50°C under stirring, and add 31.2g of allyl bromide Add it dropwise into the reaction bottle with a dropping funnel, and the dropwise addition is completed in 1.0 hour. After continuing to react at constant temperature for 29 hours, cool to room temperature, add 300 mL of water to the reaction solution, extract three times with 300 mL of ether, combine the organic phases, and separate the organic phases by rectification to obtain 46.8 g of fluorine-containing olefins with a yield of 65%.

[0047] (2) Add 120 g of fluorine-containing olefins into a 250 mL autoclave, and then add Karstede catalyst into the autoclave. The amount of Karstede catalyst used is 10 ppm of the mass of methyldichlorosilane. Seal the reaction kettle, start stirring and heating, so that the temperature of the reaction kettle rise...

Embodiment 3

[0051] (1) Put 60g of hexafluoropropylene dimer and 23.2g of potassium fluoride into a three-necked flask with a reflux condensing device, then add 30mL of anhydrous DMF, heat to 80°C under stirring, and add 20.4g of allyl bromide Add it dropwise into the reaction bottle with a dropping funnel, and the dropwise addition is completed in 1.0 hour. After continuing to react at constant temperature for 19 hours, cool to room temperature, add 300 mL of water to the reaction solution, extract three times with 300 mL of ether, combine the organic phase, and separate the organic phase by rectification to obtain 36.4 g of the product fluorine-containing olefin, with a yield of 60%.

[0052] (2) Add 120 g of fluorine-containing olefin into a 250 mL autoclave, and then add Karstede catalyst into the autoclave. The amount of Karstede catalyst used is 50 ppm of the mass of methyldichlorosilane. Seal the reaction kettle, start stirring and heating, so that the temperature of the reaction ke...

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Abstract

The invention discloses a fluoride-containing silicone oil defoamer and a preparation method thereof, the fluoride-containing silicone oil defoamer has a structural formula as shown in formula I, the method is as follows: addition reaction of hexafluoropropene dimmer and allyl bromide under the effect of potassium fluoride or cesium fluoride for preparation of fluorinated olefin, hydrosilylation reaction of the fluorinated olefin and dichloromethylsilane for preparation of fluoride-containing dichlorosilane, hydrolysis of the fluoride-containing dichlorosilane and dimethyldichlorosilane in neutral or weak alkaline condition, and final condensation polymerization of hydrolysate in alkaline conditions by use of hexamethyldisiloxane as an end-capping reagent for preparation of the fluoride-containing silicone oil defoamer. The fluoride-containing silicone oil defoamer can effectively reduce the polymer surface energy, is better in defoaming effect, can effectively reduce the solubility in the oil phase, increases the polymer high temperature resistance and chemical stability, can inhibit the foam generation in a long period, is small in dosage, simple in technical process, low in production cost, and suitable for large-scale industrial production, and the lowest concentration can be 3ppm of system concentration.

Description

technical field [0001] The invention relates to the technical field of special polymer materials in chemical synthesis, in particular to a fluorine-containing silicone oil defoamer and a preparation method thereof. Background technique [0002] In the industrial production process in the fields of petroleum, textile, paint, ink, rubber, resin and food processing, a large amount of foam is often produced, which not only occupies production space, hinders the normal operation of production machines, reduces production efficiency, and may cause fire, Safety issues such as explosions. Since Quincke, a German physicist, first proposed the idea of ​​chemical defoaming, defoamers have developed rapidly, and various new defoamers have continuously hit the market. Defoamers are recognized as the most effective method of foam elimination. In addition to requiring a fast defoaming speed in an instant, the defoamer also needs to suppress the generation of foam for a long time. At pres...

Claims

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Application Information

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IPC IPC(8): C08G77/24B01D19/04
Inventor 向德轩陈欣王树华周强
Owner ZHEJIANG JUHUA HANZHENG NEW MATERIAL
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