Preparation method of fluorine-silicon surfactant

A technology of surfactant and fluorosilicon, applied in the field of preparation of fluorosilicon surfactant, can solve the problems of small surface energy of fluorine-containing surfactant, limited application field, high production cost, and achieve low surface tension, stable reaction, Separate simple effects

Active Publication Date: 2011-05-25
JINZHOU DPF TH CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Fluorine-containing surfactants have low surface energy and have water and oil repellency, but their production costs are high, their solubility is poor, and their application fields are limited.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Add 446.1g of perfluorooctyl ethylene and 0.5g of platinum chlorate into a 1000ml four-neck flask equipped with a stirrer, condenser, thermometer, dropping funnel, and nitrogen conduit, and stir to raise the temperature to 40°C. After the temperature is stable, start to drop Add 136g of trichlorosilane, add dropwise for 1 hour, continue to react for 2 hours, obtain 570g of intermediate product after separation and filtration, add 150g of pyridine to the intermediate product and raise the temperature to 80°C, after the temperature is stable, start to drop methanol 100g, drop within 1 hour After the addition was completed, the reaction was continued for 2 hours after the dropwise addition. The exhaust gas in the reaction process was absorbed with 10% NaOH solution, and the obtained product was subjected to vacuum distillation to remove pyridine to obtain 550 g of the target product, with a yield of 97% and a purity of 99%. The measured surface tension of the glass surface ...

Embodiment 2

[0014] Add 450 g of perfluorohexylethylene and 1.0 g of platinum chlorate into a 1000 ml four-necked flask equipped with a stirrer, a condenser, a thermometer, a dropping funnel, and a nitrogen conduit, and stir to raise the temperature to 50°C. Chlorosilane 180g, dropwise adding time is 1h, continue to react for 3h, obtain intermediate product 613g after separation and filtration. Add 200g of pyridine to the intermediate product and raise the temperature to 90°C. After the temperature is stable, add 110g of methanol dropwise. The dropwise addition is completed within 0.5h. After the dropwise addition, continue to react for 0.5h. The waste gas in the reaction process is absorbed by 10% NaOH solution. The obtained product was removed by vacuum distillation to remove pyridine to obtain 590 g of the target product, with a yield of 97.2% and a purity of 98%. The measured surface tension of the glass surface treated with this product is 17 dynes / m, which has excellent anti-fouling ...

Embodiment 3

[0016] Add 500g of perfluorooctyl ethylene and 0.5g of platinum chlorate into a 1000ml four-neck flask equipped with a stirrer, condenser, thermometer, dropping funnel, and nitrogen conduit, and stir to raise the temperature to 100°C. After the temperature is stable, start to drop 160g of trichlorosilane, the dropping time is 1h, continue to react for 1h, obtain 620g of intermediate product after separation and filtration, add 180g of pyridine and raise the temperature to 120°C, after the temperature is stable, start to add 160g of ethanol dropwise, the dropwise addition is completed within 1h, dropwise After the completion, the reaction was continued for 3 hours. The waste gas in the reaction process was absorbed with 10% NaOH solution, and the obtained product was subjected to vacuum distillation to remove the solvent pyridine to obtain 661 g of the target product, with a yield of 97% and a purity of 98.5%. The measured surface tension of the glass surface treated with this p...

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Abstract

The invention discloses a preparation method of a fluorine-silicon surfactant. The method comprises the following steps of: continually dripping 13 to 18 weight parts of trichlorosilane into 44 to 65 weight parts of perfluor alkyl ethylene or perfluor alkyl ethyl iodide serving as a raw material in the presence of 0.1 to 1.0 weight part of noble metal catalyst so as to obtain an intermediate product; and adding 14.8 to 20 weight parts of high-boiling-point solvent into the intermediate product, continuously dripping 10 to 16.35 weight parts of methanol or ethanol for reacting, decompressing and rectifying so as to obtain a target product. In the method, raw materials are readily available, byproduct is not produced, a reaction in an entire synthesis process is stable, process control is stable, safety, low cost and easy separation are realized, the yield of a final fluorine-silicon surfactant is over 95 percent, and the purity of the surfactant is over 98 percent. Due to the presence of a siloxane active group, the fluorine-silicon surfactant can react with and be tightly combined with substances with a hydroxy functional group, such as glass and the like, so that the surface of the fluorine-silicon surfactant has high waterproofness, oil resistance and soil resistance, surface tension is less than 17.6 dynes per meter, and light transmittance is over 99.9 percent.

Description

technical field [0001] The invention relates to a preparation method of a fluorosilicon surfactant. Background technique [0002] Surfactants are widely used in the glass industry, automotive industry, electronics, and special surface treatment fields, requiring good waterproof, oil-proof, and rust-proof properties, as well as good anti-fingerprint, anti-fouling, and anti-fog properties. The existing surfactants mainly include hydrocarbon and fluorine-containing surfactants. Hydrocarbon surfactants have large surface energy and do not have waterproof and oil-proof properties. Fluorine-containing surfactants have low surface energy and have waterproof and oil-proof properties, but their production costs are high, their solubility is poor, and their application fields are limited. Contents of the invention [0003] The technical problem to be solved by the present invention is to provide a preparation method of a fluorosilicon surfactant with good waterproof, oil-proof, an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18B01F17/54C09K23/54
Inventor 魏潇高春风孙百开
Owner JINZHOU DPF TH CHEM CO LTD
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