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Fluoride-free waterproof agent with stereo silane structure and preparation method of fluoride-free waterproof agent

A fluorine-free water repellent, structural chain technology, applied in the direction of repelling fibers, fiber types, textiles and papermaking to liquids, etc., can solve the problems of refractory degradation, low waterproof effect, and restricting the migration of silicon atoms.

Active Publication Date: 2017-06-09
BEIJING CTA TEX CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In 2000, American manufacturers launched a plan to promote the environmental protection of fluorocarbons, and reached a consensus: by 2015, all fluorocarbons used in impregnation must meet environmental protection requirements, while traditional perfluorooctyl The degradation product of fluorine-containing finishing agents, perfluorooctane sulfonate / ester (PFOS), is currently recognized as one of the most difficult to degrade organic pollutants in the world, and has the possibility of persistence, bioaccumulation, and long-distance environmental transport , have a serious impact on human health and the living environment
However, traditional organosilicon-based fluorine-free waterproofing agents mainly use long-chain siloxane, carboxyl, amino, and epoxy-modified long-chain silicone oils, and the waterproof effect is not outstanding, mainly due to the fact that silicon atoms with low surface energy act as polymers. The existence of the main chain of the polymer restricts the migration of silicon atoms to a large extent, and most of the silicon atoms are embedded in the polymer, which greatly reduces the water repellent effect

Method used

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  • Fluoride-free waterproof agent with stereo silane structure and preparation method of fluoride-free waterproof agent
  • Fluoride-free waterproof agent with stereo silane structure and preparation method of fluoride-free waterproof agent
  • Fluoride-free waterproof agent with stereo silane structure and preparation method of fluoride-free waterproof agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0083] Embodiment 1, preparation fluorine-free waterproofing agent

[0084] according to figure 1 The flow chart shown in the preparation of fluorine-free water repellent, the specific steps are as follows:

[0085] (1) Cetyl acrylate 50g, heptaisobutylacryloxypropyl cage silsesquioxane (heptaisobutylacrylate propyl cage silsesquioxane) 15g, hydroxyethyl acrylate 5g , cetyltrimethylammonium bromide 2g, polyoxyethylene sorbitan monoglyceride 2g, acetone 26g were added to 150g deionized water, mixed with a high-speed shear machine at 3000 rpm for 5 minutes, then added Homogenize for 10 minutes in a high-pressure homogenizer with a pressure of 40 MPa to obtain a stable oil-in-water pre-emulsion.

[0086] In the above-mentioned pre-emulsion, monomer I is hexadecyl acrylate, which accounts for 20% of the emulsion, and monomer II is heptaisobutylacryloyloxypropyl cage silsesquioxane (heptaisobutylacrylate propyl cage Type silsesquioxane), accounting for 6% of the emulsion, monome...

Embodiment 2

[0089] Embodiment 2, preparation fluorine-free waterproofing agent

[0090] according to figure 1 The flow chart shown in the preparation of fluorine-free water repellent, the specific steps are as follows:

[0091] (1) Cetyl acrylate 50g, heptaisobutylmethacryloxypropyl cage silsesquioxane (heptaisobutylmethacrylate propyl cage silsesquioxane) 15g, hydroxyethyl acrylate 2.5g g, N-methylolacrylamide 2.5g, octadecyltrimethylammonium bromide 4.2g, lauryl polyoxyethylene (10) ether 2.8g, methyl ethyl ketone 18g were added to 155g deionized After mixing in water with a high-speed shearer at 3000 rpm for 5 minutes, add it to a high-pressure homogenizer with a pressure of 40 MPa and homogenize for 10 minutes to obtain a stable oil-in-water pre-emulsion.

[0092]In the above-mentioned pre-emulsion, monomer I is hexadecyl acrylate, which accounts for 20% of the emulsion, and monomer II is heptaisobutylmethacryloxypropyl cage silsesquioxane (heptaisobutylmethacrylic acid propyl group...

Embodiment 3

[0095] Embodiment 3, preparation fluorine-free waterproofing agent

[0096] according to figure 1 The flow chart shown in the preparation of fluorine-free water repellent, the specific steps are as follows:

[0097] (1) 57.5g of octadecyl acrylate, 5g of heptaisobutylacryloxypropyl cage silsesquioxane (heptaisobutylacrylate propyl cage silsesquioxane), 5g of N-methylol Add 7.5g of methacrylamide, 2g of octadecyltrimethylammonium bromide, 3g of polyoxyethylene sorbitan monoglyceride, and 25g of dipropylene glycol into 150g of deionized water, and use a high-speed shear at 3000 rpm After cutting and mixing for 5 minutes, it was added to a high-pressure homogenizer with a pressure of 40 MPa and homogenized for 10 minutes to obtain a stable oil-in-water pre-emulsion.

[0098] In the above-mentioned pre-emulsion, monomer I is octadecyl acrylate, which accounts for 23% of the emulsion, and monomer II is heptaisobutylacryloyloxypropyl cage silsesquioxane (heptaisobutylacrylate prop...

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Abstract

The invention discloses a fluoride-free waterproof agent with a stereo silane structure and a preparation method of the fluoride-free waterproof agent. In a formula I of a polymer, R1 refers to a long-chain acrylate structural chain segment, R2 refers to a polyhedral oligomeric silsesquioxane structural chain segment, R3 refers to a functional monomer structural chain segment, X refers to a natural number in a range of 1-150, and Y and Z refer to natural numbers in a range of 1-100. The fluoride-free waterproof agent is aqueous emulsion of the polymer shown as the formula I. By adoption of a polyhedral oligomeric silsesquioxane monomer with a vinyl structure for preparation of the fluoride-free waterproof agent through microemulsion polymerization, introduction of polyhedral oligomeric silsesquioxane with a stereo structure to a lateral group of a polymer long chain is realized, a low-surface-energy siloxane cubic structure can migrate to the fabric fiber surface more effectively in an emulsion film forming spread process to form continuous projections on the fabric fiber surfaces, and consequently waterproof effects are greatly improved. The fluoride-free waterproof agent is an environment-friendly waterproof agent, free of biotoxicity and nondegradability and harmless to organisms and environment.

Description

technical field [0001] The invention relates to a fluorine-free waterproofing agent with a three-dimensional silane structure and a preparation method thereof. Background technique [0002] In the early 1970s, driven by the new technological revolution, the rapidly developing industrial countries led by the United States gradually realized the importance of protecting the environment. The establishment of various environmental protection organizations and the improvement of laws and regulations have restricted the development of certain industries to varying degrees, but they have also largely guaranteed the sustainable development of the earth's ecosystem. In 2000, American manufacturers launched a plan to promote the environmental protection of fluorocarbons, and reached a consensus: by 2015, all fluorocarbons used in impregnation must meet environmental protection requirements, while traditional perfluorooctyl The degradation product of fluorine-containing finishing agen...

Claims

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Application Information

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IPC IPC(8): C08F283/12C08F220/18C08F220/28C08F220/58C08F220/32C08F220/34C08F2/30C08F2/28D06M15/356D06M101/06D06M101/32D06M101/34
CPCC08F2/28C08F2/30C08F283/124D06M15/3568D06M2101/06D06M2101/32D06M2101/34D06M2200/12C08F220/1818
Inventor 李翔高殿权李建华张卫玲邵颖
Owner BEIJING CTA TEX CHEM
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