Fluorine-containing silicone oil and preparation method thereof

A technology of fluorine-containing silicone oil and amino silicone oil, which is applied in textiles and papermaking, fiber treatment, plant fiber, etc., can solve the problems of high cost and high production cost, and achieve the effects of overcoming yellowing, increasing added value, and ensuring quality

Inactive Publication Date: 2012-08-15
SUZHOU UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are quaternary ammonium cationic groups in the quaternary ammonium salt type modified amino silicone oil, and its compatibility and ionic stability must be considered when it is formulated into a finishing working solution; high cost is also another important factor limiting its large-scale use. At present, Most of the organic silicon quaternary ammonium antibacterial finishing agents used in China are imported from abroad, and the production cost is high

Method used

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  • Fluorine-containing silicone oil and preparation method thereof
  • Fluorine-containing silicone oil and preparation method thereof
  • Fluorine-containing silicone oil and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Synthesis of fluorine-containing silicone oil: Add 81.8g of hexafluorobutyl methacrylate, 100g of aminopropyl silicone oil and 80g of tetrahydrofuran into a 2L three-necked flask equipped with mechanical stirring and nitrogen protection device, pass through nitrogen protection, stir and heat up to 50°C for reaction 4 hours, its reaction formula is:

[0030]

[0031] Among them, m is 15, n is 8;

[0032] After the reaction was completed, the solvent was distilled off to obtain hexafluorobutyric acid isopropylamino-modified amino silicone oil with a yield of 91%. The fluorine content of the product was 25%. FT-IR (v, cm -1 ): 3301.1cm -1 (-NH 2 ), 2963.9 (-CH 3 ), 1730.0 (C=0), 1384.2, 1188.9 (C-F), 1063.3, 1091.9 (Si-C-Si), 1260.0, 801.8 (Si-CH 3 ).

[0033] See attached figure 1, it is the infrared spectrogram of the hexafluorobutoxyamidoisopropylamine-modified amino silicone oil prepared according to the technical scheme of this embodiment, and is compared w...

Embodiment 2

[0038] Synthesis steps: Add 8.26g of dodecafluoroheptyl methacrylate, 50g of aminoethyl silicone oil and 80g of tetrahydrofuran into a 2L three-necked flask equipped with mechanical stirring and nitrogen protection device, pass through nitrogen protection, stir and heat up to 40°C for 5 hours , whose reaction is:

[0039]

[0040] Among them, m is 12, n is 6;

[0041] After the reaction, the solvent was distilled off to obtain dodecafluoroheptyloxyisopropylamino-modified amino silicone oil with a yield of 85%. The fluorine content of the product was 12%. FT-IR (v, cm -1 ): 3309cm -1 (-NH 2 ), 2975.1 (-CH 3 ), 1738.0 (C=0), 1386.6, 1191.3 (C-F), 1065.2, 1093.2 (Si-C-Si), 1265.2, 802.8 (Si-CH 3 ).

[0042] Preparation of finishing working solution: In a 500mL tall beaker, add 200g of water, 2g of polyethylene glycol, 6g of sodium lauryl sulfate and 4g of Tween80, and stir to dissolve. Under high-speed stirring, 40 g of the above-prepared dodecafluoroheptyloxyisopropyl...

Embodiment 3

[0047] Synthesis steps: Add 10.32g of dodecafluoroheptyl acrylate, 50g of aminopropyl silicone oil and 80g of toluene into a 2L three-necked flask equipped with mechanical stirring and nitrogen protection device, pass through nitrogen protection, stir and heat up to 60°C for 4 hours, and the reaction The formula is:

[0048]

[0049] Among them, m is 8, n is 9;

[0050] After the reaction was completed, the solvent was distilled off to obtain dodecafluoroheptyloxyacylamide-modified amino silicone oil with a yield of 88%. The fluorine content of the product was 15%. FT-IR (v, cm -1 ): 3311.1cm -1 (-NH 2 ), 2975.4 (-CH 3 ), 1738.5 (C=0), 1388.1, 1194.2 (C-F), 1065.5, 1093.8 (Si-C-Si), 1265.5, 805.8 (Si-CH 3 ).

[0051] Preparation of finishing working solution: In a 500mL tall beaker, add 200g of water, 2g of polyethylene glycol, 8g of sodium lauryl sulfate and 8g of Tween80, and stir to dissolve. Under high-speed stirring, 40 g of the above-prepared dodecafluorohepty...

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Abstract

The invention relates to fluorine-containing silicone oil and a preparation method thereof. Fluorine-containing alcoxyl acylpropyl amine-modified amino silicone oil is prepared by introducing a fluorine-containing alcoxyl acylpropyl amine substituent into a side chain of the amino silicone oil by addition reaction of unsaturated double bond on fluorine-containing alkyl acrylic ester or fluorine-containing alkyl methacrylic ester and an amino group on a side group of the amino silicone oil. Fabric finishing working liquid with high stability is obtained by emulsifying the fluorine-containing alcoxyl acylpropyl amine-modified amino silicone oil provided by the invention; by applying the fluorine-containing alcoxyl acylpropyl amine-modified amino silicone oil to finishing cotton fabric by a rolling-baking-roasting finishing process, the obtained cotton fabric has good soft effect; and due to the introduction of a fluoroalkyl group into the side chain of the amino silicone oil, soft finishing of the fabric and multifunctional finishing for endowing the fabric with water-proof performance, oil-proof performance and the like are realized, the defect that the fabric turns yellow easily when being finished with the conventional amino silicone oil is also overcome, the quality of the fabric is guaranteed, and the added value of the product is also improved.

Description

technical field [0001] The invention relates to a fluorine-containing silicone oil and a preparation method thereof, in particular to a fluorine-containing alkoxyamidopropylamine-modified amino silicone oil and its synthesis technology. The product is formulated into an emulsion and applied to textile finishing. Background technique [0002] Because of its essential softness, amino silicone oil has been widely used in fabric softening and finishing, which can make cotton, linen, silk, wool, polyester, acrylic, polypropylene and nylon fabrics soft, smooth, soft and elastic. The most important problem in the application process is that the side chain amino group has poor thermal stability and anti-oxidation stability, and oxidation side reactions are prone to occur during the high-temperature finishing process, resulting in yellowing of the fabric. [0003] For the above-mentioned shortcomings of amino silicone oil, it is generally considered that acylation modification is a m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/385D06M15/657D06M101/06
Inventor 李战雄周绍强陈国强蔡建和卢艳光杜丽萍
Owner SUZHOU UNIV
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