Preparation and application of perfluoro-short-carbon-chain-containing water-repellent oil-repellent finishing agent

A perfluorinated short carbon chain, water-repellent and oil-repellent technology, which is applied in fiber processing, textiles, papermaking, plant fibers, etc., can solve the problems of short carbon chains and lack of oil repellency, and achieve good stability, good air permeability, The effect of simple finishing process

Inactive Publication Date: 2013-11-27
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Perfluorinated short carbon chain (n<8) compounds will not cause problems similar to PFOS, and perfluorocarbon chain compounds have good water repellency and oil repellency. Studies have sh

Method used

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  • Preparation and application of perfluoro-short-carbon-chain-containing water-repellent oil-repellent finishing agent
  • Preparation and application of perfluoro-short-carbon-chain-containing water-repellent oil-repellent finishing agent
  • Preparation and application of perfluoro-short-carbon-chain-containing water-repellent oil-repellent finishing agent

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0031] Example 1

[0032] Preparation of perfluorinated short carbon chain acrylic monomers:

[0033] Dissolve the crude cuprous chloride solid in concentrated hydrochloric acid, then dilute it with distilled water to obtain a white precipitate, filter it, wash it with water three times, wash it several times with absolute ethanol and absolute ether, and dry it for later use.

[0034] Add 4.85g (0.01mol) of dry N-propyl-N-hydroxyethylperfluorohexylsulfonamide to a 100mL three-necked flask, then add 0.05g of newly prepared cuprous chloride and 2.26g (0.025mol) of triethylamine , and then add half the amount of chloroform 15mL to make the three miscible, and the system is a green opaque mixture. The remaining 15 mL of chloroform was mixed with 2.53 g (0.025 mol) of acryloyl chloride, and slowly added to the three-necked flask under ice-bath conditions. During the addition of acryloyl chloride, the temperature in the three-necked flask was kept at 0-5°C.

[0035] After all the ...

Example Embodiment

[0037] Example 2

[0038] Preparation of fluorine-containing finishing agent:

[0039] Dissolve 6.14g (11.4mmol) of fluorine-containing acrylic acid monomer, 1.176g (3.6mmol) of stearyl acrylate and 0.056g (0.479mmol) of propylene-2-hydroxyethyl ester in 5mL of acetone with semi-emulsifier (OP-100.132 g; SDS0.074g) were added together into a single-necked flask, heated to 50°C, pre-emulsified for 30 minutes, and used as a pre-emulsified monomer for later use.

[0040]Then add 40mL of water and the remaining half of the emulsifier (OP-100.132g; SDS0.074g) into the three-necked flask, raise the temperature to 50°C, pre-emulsify for 30min, then raise the temperature to 70°C, add half of the initiator APS0.0183g, 4~5min Finally, add 1 / 2 of the spare pre-emulsified monomer in the single-necked flask, and after 0.5h of reaction, add the remaining 1 / 2 pre-emulsified monomer in the single-necked flask. And at the same time slowly add the remaining initiator APS0.0183g. After the dr...

Example Embodiment

[0041] Example 3

[0042] Take an appropriate amount of the emulsion-like finishing agent prepared in Example 2, immerse the pure cotton fabric in the emulsion for 30 minutes, after two dipping and two padding (liquid retention rate 80%), pre-dry at 100°C for 2 minutes, and then dry at 160°C Bake for 2 minutes and cool to room temperature. The water resistance test is carried out according to 3M-II-1988, and the oil resistance test is carried out according to AATCC118-2002. The waterproof level of the fabric is 6, and the oil resistance level of the fabric is 3.

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Abstract

The invention relates to a preparation method of a perfluoro-short-carbon-chain-containing water-repellent oil-repellent finishing agent, which comprises the following steps: preparing N-propylperfluorohexylsulfamidoethylacrylate; dissolving fluorine-containing acrylic acid monomer, octadecyl acrylate and propylene-2-hydroxyethyl ester in a solvent to obtain a monomer mixed solution, adding half of emulsifier into the monomer mixed solution to carry out pre-emulsification, thereby obtaining a pre-emulsification monomer; carrying out pre-emulsification on water and the rest half of emulsifier, heating to 65-90 DEG C, adding half of initiator solution, adding half of pre-emulsification monomer after 4-5 minutes to react, adding the rest half of pre-emulsification monomer while slowly adding the rest of initiator, continuing the reaction for 4-8 hours after dropwise addition is finished, cooling to room temperature after the reaction is finished, and filtering to obtain the finishing agent. The finishing agent has high stability, and is free of restricted components which are harmful to the human body and environment; and the finished fabric has favorable water repellency, oil repellency and anti-fouling property.

Description

technical field [0001] The invention belongs to the field of preparation and application of fabric auxiliary finishing agents, and in particular relates to the preparation and application of a water- and oil-repellent finishing agent containing fluorine short carbon chains. Background technique [0002] Fluorine-containing compounds have many excellent properties, such as excellent surface properties, high chemical stability, thermal stability, aging resistance, water and oil repellency, etc. Since the American 3M Company developed the waterproof, oil-proof and anti-fouling fluorine-containing finishing agent named Scotchguard in 1956, the fluorine-containing finishing agent has attracted great interest because of its advantages of high efficiency, stability, corrosion resistance and friction resistance. be continuously developed. Since the 1980s, fluorine-containing (meth)acrylate polymer emulsion has become the mainstream product of "three-proof" finishing at home and abr...

Claims

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Application Information

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IPC IPC(8): C08F220/38C08F220/18C08F220/28C08F2/30C08F2/26D06M15/277D06M101/06
Inventor 林苗杨勇李晓伟张丽媛
Owner DONGHUA UNIV
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