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A kind of perfluoroalkyl polyacrylate waterproofing agent, preparation method and application

A technology of perfluoroalkyl polyacrylate and perfluoroalkyl acrylate, which can be used in textiles and papermaking, fiber treatment, and liquid-repellent fibers, etc. The chain segments are easy to reorient, dump, and the matrix structure is exposed, etc., to achieve excellent waterproof effect, superior liquid repellency, and stable surface conformation

Active Publication Date: 2017-11-03
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In recent years, there have been many research reports on the synthesis and application of short fluorocarbon chain compounds at home and abroad. It has been found that the short carbon chain perfluoroalkyl groups on the surface of the fluorine film have low rigidity and no crystallinity, and cannot form a stable liquid crystal structure arrangement. The fluorocarbon chain segment of the short carbon chain fluoroalkyl protective film is easy to reorient and fall after contacting the liquid, which easily exposes the matrix structure and makes the fluorine film shielding invalid, that is, the so-called short carbon chain perfluoroalkyl "surface reconstruction" occurs. ”, resulting in a pendant terminal trifluoromethyl group (-CF 3 ) layer is damaged or even collapsed, so the effective liquid repellent function cannot be achieved

Method used

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  • A kind of perfluoroalkyl polyacrylate waterproofing agent, preparation method and application
  • A kind of perfluoroalkyl polyacrylate waterproofing agent, preparation method and application
  • A kind of perfluoroalkyl polyacrylate waterproofing agent, preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] 1. Synthesis of 1H, 1H, 2H, 2H-7-thia-perfluoroundecyl methacrylate

[0059] a. 46.9g of nonafluorobutyl tetrafluorosulfur bromide, 0.40g of di-tert-butyl peroxide, 0.4g of calcium carbonate and 48g of 1,3-bis(trifluoromethyl)benzene solvent were added to the reaction kettle, sealed, After evacuation, nitrogen was filled to replace the air in the reaction kettle, and then evacuation was carried out to replace. A total of 4 replacements. After being warming up to 45 ℃, tetrafluoroethylene is passed into this reactor for insulation, stirring reaction, and the control stirring rate is 55 rev / min, the feeding speed of tetrafluoroethylene is 12g / hour, and the pressure is 0.48MPa, and stops after 2 hours Tetrafluoroethylene was introduced, and the reaction was continued for 2 hours. After cooling, 1,3-bis(trifluoromethyl)benzene was removed from the reaction mixture by distillation under reduced pressure. The product thiaperfluorononyl bromide is obtained.

[0060] b. 65....

Embodiment 2

[0077] 1. Synthesize 1H, 1H, 2H, 2H-7-thia-perfluoroundecyl methacrylate according to Example 1

[0078] 2. Monomer pre-emulsion preparation

[0079] a. Add 1H, 1H, 2H, 2H-7-thia-perfluoroundecyl methacrylate 28.8g, 18.1g butyl acrylate, 9.1g methyl methacrylate and 2.6g to the tall beaker in turn g hydroxyethyl methacrylate is mixed to obtain a monomer mixture with good uniformity and fluidity.

[0080] b. Add 0.8g nonionic surfactant AEO-6 and 0.8g part cationic surfactant octadecyltrimethylammonium bromide into 110 parts deionized water, stir to dissolve, then add the above monomer mixture, 8000 High-speed shearing and stirring at rpm for 15 minutes to obtain a monomer pre-emulsion.

[0081] 3. Polymerization

[0082] a. Dissolve 0.7g of ammonium persulfate in 20g of deionized water to obtain an initiator solution for use.

[0083] b. Add the prepared monomer pre-emulsion into the reactor, heat it to 78°C, slowly add the prepared initiator solution dropwise, the droppin...

Embodiment 3

[0093] 1. Synthesis of 1H,1H,2H,2H-7-thia-perfluoroundecyl acrylate

[0094] a. Add 45.8g of nonafluorobutyltetrafluorosulfur bromide, 0.5g of dibenzoyl peroxide, 0.4g of calcium carbonate and 55g of trifluorotoluene solvent into the reaction kettle, seal it, vacuumize it, and fill it with nitrogen for replacement The air in the reactor was vacuumed and replaced. A total of 4 replacements were performed. After heating up to 45°C, feed tetrafluoroethylene into the reactor to keep warm and stir to react, control the stirring rate to 60 rpm, the feeding speed of tetrafluoroethylene to 13g / hour, the pressure to 0.50MPa, stop after 2 hours Tetrafluoroethylene was introduced, and the reaction was continued for 3 hours. After cooling, the reaction mixture was distilled off under reduced pressure to remove benzotrifluoride. The conditions of the reduced pressure distillation were a temperature of 50° C. and a vacuum degree of 20 mmHg. The product thiaperfluorononyl bromide was obta...

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Abstract

The invention discloses a perfluoroalkyl polyacrylate waterproofing agent, a preparation method and an application. The active ingredient of the waterproofing agent is sulfur-containing long heterochain perfluoroalkyl acrylate copolymer, and sulfur-containing long heterochain perfluoroalkyl acrylate, butyl acrylate, methyl methacrylate and hydroxyethyl methacrylate Composition of mixed monomers, under the emulsification of non-ionic surfactants and anionic surfactants, it is obtained by initiating emulsion polymerization with an initiator. Applying this finishing agent to cotton fabric finishing can provide very excellent waterproof function. Due to the crystallinity of sulfur-containing long heterochain perfluoroalkyl groups, there is no surface reconstruction phenomenon when the acrylate copolymer contacts liquid, and the waterproof function is excellent. Moreover, long heterochain perfluoroalkyl groups contain carbon-sulfur heterobonds, are easy to degrade, and have no cumulative toxicity, so they are not banned fluorine-containing chemicals. At the same time, the waterproofing agent provided by the invention is prepared by traditional emulsion copolymerization, has mild reaction conditions, low equipment requirements, simple process, easy control, and is suitable for industrial production.

Description

technical field [0001] The invention relates to a perfluoroalkyl polyacrylate waterproofing agent, a preparation method and its application, in particular to a sulfur-containing long heterochain perfluoroalkyl polyacrylate emulsion and a preparation method thereof, which are applied to fabric waterproofing Finishing belongs to the field of fine chemicals and textile chemical auxiliaries. Background technique [0002] In the process of research on the waterproof and oil-proof finishing of fabrics, it was found that treating fabrics with fluorine-containing alkyl compounds can endow fabrics with excellent waterproof properties. After decades of research and development, fluorine-containing fabric finishing agents have been commercialized and occupy a large market. The development of these fluorine-containing fabric finishing agents has greatly enriched the research field of organic fluorine materials and has become an important branch. It has received great attention from res...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F220/38C08F220/18C08F220/14C08F220/28C08F2/30C08F2/28D06M15/277D06M101/06
CPCC08F2/28C08F2/30C08F220/38C08F220/382D06M15/277D06M2101/06D06M2200/12C08F220/1804C08F220/14C08F220/281
Inventor 李战雄袁艳华
Owner SUZHOU UNIV
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