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Preparation method of (sesqui) siloxane hybrid modified fluorinated polyacrylate emulsion

A technology of fluorinated polyacrylate and acrylate, which is applied in the field of preparation of modified fluorinated polyacrylate emulsion, can solve the problems of unsatisfactory fabric stiffness and poor storage stability of emulsion, etc.

Active Publication Date: 2013-11-27
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, we found in the research that the use of a large amount of functional adhesion-enhancing monomers can easily lead to transitional crosslinking of the system, causing the storage stability of the emulsion to deteriorate; The stiffness of the finished fabric is not ideal and needs to be improved

Method used

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  • Preparation method of (sesqui) siloxane hybrid modified fluorinated polyacrylate emulsion
  • Preparation method of (sesqui) siloxane hybrid modified fluorinated polyacrylate emulsion
  • Preparation method of (sesqui) siloxane hybrid modified fluorinated polyacrylate emulsion

Examples

Experimental program
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Effect test

preparation example Construction

[0033] Preparation of epoxy polyether based (silsesquioxane) crosslinking agent

[0034] see figure 1 , take EPOS-1A as an example. In a three-necked flask equipped with a thermometer and a reflux condenser, add 24.1g of tetramethylcyclotetrasiloxane (D 4 H ) and 168.0g a / b=7:1, M n = 400 allyl polyoxyethylene polyoxypropylene epoxy ether (APEE), stirring and heating to 80 ° C, then adding 50 ppm platinum catalyst, after the system turns transparent, continue to stir and react for 10 minutes to obtain a transparent liquid, namely epoxy poly Ether-based siloxane crosslinking agent EPOS-1A.

[0035] The preparation method of other epoxy polyether-based (silsesquioxane) siloxane crosslinking agents is the same as that of EPOS-1A, and its raw material consumption is shown in Table 1.

[0036] Table 1 prepares the used raw material and consumption thereof of epoxy polyether base (silsesqui) siloxane EPOS

[0037]

[0038] APEE (1) : a / b=7:1, M n = 400; APEE (2) : a=10, ...

Embodiment 1

[0039] Example 1: Weighing 37.5g of the structure as CH in turn 2 =CHCOOCH 2 CH 2 (CF 2 ) 4～12 CF 3 Perfluoroalkane ethyl acrylate, 10.0g lauryl methacrylate, 1.5g hydroxypropyl acrylate and 0.5g 4-chloromethylstyrene and 0.5g vinyltriethoxysilane were mixed to form Oil phase monomer mixture. Then, weigh 0.7g of mercaptoethanol, 2.5g of cetyltrimethylammonium chloride 1631, 1.5g of fatty alcohol polyoxyethylene ether and 163.2g of deionized water and mix them with the oil phase monomer mixture, and mix them evenly with mechanical stirring , and then ultrasonically emulsified at 30±2° C. for 30 minutes to make a stable pre-emulsion, which is recorded as component (I), placed in the dropping funnel (I), and set aside.

[0040] Another 1.5 g of ammonium persulfate was dissolved in 30.0 g of deionized water to make an aqueous initiator solution, which was recorded as component (II), and placed in the dropping funnel (II) for subsequent use.

[0041] In the four-neck flask e...

Embodiment 2

[0042] Example 2: Weigh 20.0g dodecafluoroheptyl methacrylate, 20.0g lauryl acrylate, 2.5g butyl acrylate, 3.0g N-methylolacrylamide, 2.0g 4-chloromethylbenzene Ethylene and 2.5g of γ-methacryloxypropyltrimethoxysilane were mixed to form the oil phase monomer mixture. Then, weigh 0.3g dodecyl mercaptan, 2.0g dodecyl dimethyl benzyl ammonium bromide and 3g fatty acid polyoxyethylene ether ester SG-10 and 211.2g deionized water and mix with oil phase monomer mixture , mechanically stirred and mixed, emulsified at 25° C. for 30 minutes with ultrasonic waves to make a stable pre-emulsion, recorded as component (I), placed in the dropping funnel (I), and set aside.

[0043] Take another 0.25g water-soluble azo initiator AV-40, dissolve it with 10.0g deionized water to make an aqueous solution of initiator, record it as component (II), place it in the dropping funnel (II), and set aside.

[0044] In the four-neck flask equipped with thermometer, reflux condenser, dropping funnel (I...

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Abstract

The invention discloses a preparation method of an epoxy polyether-based (sesqui) siloxane hybrid modified fluorinated polyacrylate emulsion, which comprises the following steps of: under the effect of cationic / nonionic or anionic / nonionic surfactants, firstly carrying out seeded emulsion copolymerization on perfluoroalkyl(methyl) acrylate, aliphatic long carbon chain (methyl) acrylate, reactive vinyl monomer and alpha-alkenyl alkoxysilane in an aqueous phase so as to synthesize a silanized long carbon chain fluorinated polyacrylate emulsion; cooling to room temperature; regulating a pH value of the system to be 5.0-6.0; adding an epoxy polyether-based (sesqui) siloxane cross-linking agent and a stiffening agent; continuously stirring for 30 min; and obtaining the (sesqui) siloxane hybrid modified fluorinated polyacrylate emulsion after filtering. The modified fluorinated polyacrylate emulsion disclosed by the invention can be used for after-treatment of textiles after dilution, so that the stiff handfeel of textiles can be improved, and an excellent water-repellent and oil-repellent performance is given to the textiles.

Description

technical field [0001] The invention relates to a preparation method of a modified fluorinated polyacrylate emulsion, in particular to a preparation method of a hybrid modified fluorinated polyacrylate emulsion with epoxy polyether group (sesqui)siloxane. Background technique [0002] Fluorinated polyacrylate (abbreviated as organic fluorine) has low surface energy and excellent water and oil repellency. It is used in the post-treatment of fiber substrates. It can not only improve the surface properties and feel of the substrate, but also endow the substrate with ideal repellency. Water-repellent and self-cleaning, without affecting the hygienic, air-permeable and moisture-permeable properties of the substrate, it can be widely used in the functional finishing of various fiber fabrics, paper and leather waterproofing, fabric coating and other aspects. [0003] Emulsion copolymerization is one of the most commonly used effective methods for the synthesis of fluorinated polyac...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F220/24C08F220/22C08F220/18C08F220/28C08F212/14C08F220/58C08F230/08C08F2/24C08F8/42C08J3/24
Inventor 安秋凤许伟马丽
Owner SHAANXI UNIV OF SCI & TECH
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