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A kind of water-based fluorine-containing water-repellent and oil-repellent agent and preparation method thereof

A water- and oil-repellent and water-based technology, which is applied in the field of water-based fluorine-containing water- and oil-repellent and its preparation, and achieves the effects of easy use, excellent water- and oil-repellent performance, and good mechanical stability.

Active Publication Date: 2016-01-20
太仓中化环保化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is no report on the preparation method of a heat-reactive fluorine-containing water-based polyurethane water and oil repellent with excellent water and oil repellency.

Method used

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  • A kind of water-based fluorine-containing water-repellent and oil-repellent agent and preparation method thereof
  • A kind of water-based fluorine-containing water-repellent and oil-repellent agent and preparation method thereof
  • A kind of water-based fluorine-containing water-repellent and oil-repellent agent and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] (1) Synthesis of fluorocarbon alkyl ester diols

[0035] Add 90g of perfluorohexyl ethanol, 40g of 2,2-dimethylolpropionic acid, 3.9g of p-toluenesulfonic acid and 130g of toluene into the reactor equipped with a stirrer and a thermometer, stir and dissolve, then raise the temperature to 140°C to make the reaction The device is in a reduced pressure state (0~-0.05MPa), reacted for 6 hours while slipping off the water, after cooling, neutralized, washed with water, distilled under reduced pressure, and refined to obtain 93.8g of light yellow viscous liquid perfluorohexyl ethyl ester binary alcohol.

[0036] 2) Synthetic water-based fluorine-containing water and oil repellent

[0037] Under nitrogen protection, 40 g of perfluorohexyl ethyl ester diol, 61.55 g of isophorone diisocyanate, 50 g of octadecyloxypropane 1,2-diol, 2,2 - Add 5g of dimethylolpropionic acid and three drops of dibutyltin dilaurate into the reaction vessel, react at 70-75°C for 6 hours to form a pr...

Embodiment 2

[0039] (1) Synthesis of fluorocarbon alkyl ester diols

[0040] Add 90g of perfluorohexyl ethanol, 40g of 2,2-dimethylolpropionic acid, 3.9g of p-toluenesulfonic acid and 130g of toluene into the reactor equipped with a stirrer and a thermometer, stir and dissolve, then raise the temperature to 140°C to make the reaction The device is in a reduced pressure state (0~-0.05MPa), reacted for 6 hours while slipping off the water, after cooling, neutralized, washed with water, distilled under reduced pressure, and refined to obtain 93.8g of light yellow viscous liquid perfluorohexyl ethyl ester binary alcohol.

[0041] (2) Synthetic water-based fluorine-containing water and oil repellent

[0042] Under nitrogen protection, 60 g of perfluorohexyl ethyl ester diol, 61.6 g of toluene diisocyanate, 30 g of octadecyloxypropane 1,2-diol, 2,2-dihydroxy Add 8g of methacrylic acid and three drops of dibutyltin dilaurate into the reaction vessel, react at 60-65°C for 5 hours to form a prepoly...

Embodiment 3

[0044] (1) Synthesis of fluorocarbon alkyl ester diols

[0045] Add 91g of perfluorohexyl ethanol, 55.6g of 2,2-dimethylolbutyric acid, 7.3g of p-toluenesulfonic acid and 145g of toluene into a reactor equipped with a stirrer and a thermometer, stir and dissolve, then raise the temperature to 140°C to make The reactor is in a reduced pressure state (0~-0.05MPa), react for 5 hours while slipping off the water, after cooling, neutralize, wash with water, distill under reduced pressure, and refine to obtain 101.6g of light yellow viscous liquid perfluorohexyl ethyl ester di Alcohols.

[0046] (2) Synthetic water-based fluorine-containing water and oil repellent

[0047] Under the protection of nitrogen, 70g of perfluorohexyl ethyl ester diol, 75.9g of toluene diisocyanate, 40g of hexadecyloxypropane 1,2-diol, 2,2-dihydroxy Add 12.5g of methyl butyric acid and three drops of dibutyltin dilaurate into the reaction vessel, react at 60-65°C for 5 hours to form a prepolymer, add a s...

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PUM

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Abstract

The invention relates to an aqueous fluoride-containing hydrophobic oil-repellent agent and a preparation method thereof. The preparation method comprises the following steps: performing an esterification reaction between fluorocarbon alkyl monohydric alcohol and 2,2-dimethylolpropionic acid or 2,2-dimethylolbutanoicacid in the presence of a catalyst 1 and an organic solvent 1 so as to generate fluorocarbon alkyl ester-based dihydric alcohol; then performing a polymerization reaction among fluorocarbon alkyl ester-based dihydric alcohol, diisocyanate, hydrocarbons-aliphatic dihydric alcohol and dihydric alcohol which contains water soluble groups in the presence of a catalyst 2 so as to generate a prepolymer; treating the prepolymer with a neutralizer and an end-capping reagent so as to obtain the aqueous fluoride-containing hydrophobic oil-repellent agent. The aqueous fluoride-containing hydrophobic oil-repellent agent is of a self-emulsifying type, has good mechanical stability and realizes effective improvement of the hydrophobic oil-repellent performance. The aqueous fluoride-containing hydrophobic oil-repellent agent not only can be used for treating various fiber products but also can be used for preparing antifouling paints for hard surfaces such as inner and outer walls, marine paints and the coatings for ceramics, bricks, woods and the like.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a water-based fluorine-containing water and oil repellent agent and a preparation method thereof. Background technique [0002] Fluorine-containing polymers have many excellent properties, such as excellent water and oil repellency. Copolymers of fluorinated alkyl (meth)acrylates and alkyl (meth)acrylates are widely used in the preparation of fluorine-containing water and oil repellents. Although the effect of fluorine-containing water and oil repellents on the market is satisfactory under certain application conditions, the polymerization process is relatively complicated, and emulsifiers with excellent performance need to be selected, which increases the difficulty of synthesis. In addition, in high and low temperature, high acid and alkali, high shear and other environments or if the storage time is too long, the emulsion will flocculate or precipitate, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G18/38C08G18/32C08G18/83D06M15/576C09D175/04
CPCC08G18/0823C08G18/3812C08G18/8016C08G18/8019C08G18/8048C08G18/8054C08G18/831C09D175/04D06M15/576D06M2101/06D06M2101/32D06M2101/34D06M2200/11D06M2200/12
Inventor 朱敏梁成锋顾子旭李进李全义纪敏
Owner 太仓中化环保化工有限公司
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