Acrylamide copolymer containing halothane and phosphoric acid ester as well as preparation method and application thereof

A technology of acrylamide copolymer and fluorine-containing alkyl phosphonate, which is applied in the direction of plant fiber, textile and papermaking, fiber treatment, etc., and can solve the problems of different fabric properties and other changes

Inactive Publication Date: 2010-09-15
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the combination of two finishing agents has to face the problem of compatibility of finishing agents. The performance of the final product may be different fr

Method used

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  • Acrylamide copolymer containing halothane and phosphoric acid ester as well as preparation method and application thereof
  • Acrylamide copolymer containing halothane and phosphoric acid ester as well as preparation method and application thereof
  • Acrylamide copolymer containing halothane and phosphoric acid ester as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] CH of anhydrous tert-butanol (0.5mol, 68.66g) 2 Cl 2 (50mL) solution was added dropwise under ice bath conditions (0°C-5°C) in CH 2 Cl 2 (100mL) solution, the dropwise addition is completed, after continuing the reaction at 0°C--5°C for 1h, add trifluoroethanol (1mol, 100.04g) dropwise in CH 2 Cl 2 (50 mL) solution. After completion of the dropwise addition, warm up to room temperature and react overnight (12h), heat to reflux for 3h and distill under reduced pressure to collect the fraction at 62°C / 10mmHg, which is difluoroalkoxyphosphonic acid. Gas-mass spectrometer, data analysis and characterization are as follows:

[0052] 1 HNMR (400MHz, CDCl3 ) : δ4.46(m, 4H), 7.04(d, J=755.6, H).

[0053] 19 F NMR (376MHz, CDCl 3 ): δ-74.8(m, 6F).

[0054] GC-MS m / z (EI, 70ev): 247[M+1]. +

[0055] IR (thin film, cm -1 ): 1460, 1420, 1285, 1175, 1110, 993, 845.

Embodiment 2

[0057] A solution of bisfluoroalkoxyphosphonic acid (117.9 g, 0.48 mol) in anhydrous acetonitrile (80 mL) was added at one time to trichloroisocyanuric acid (37.2 g, 0.16 mol) in anhydrous acetonitrile (240 mL), and the reaction solution Stir at room temperature for about 10 minutes, after a white precipitate appears, stir for another 5 minutes, filter the reaction solution, remove the solvent, and collect fractions at 62°C / 10mmHg by distillation under reduced pressure. Colorless fuming liquid bisfluorinated alkoxyphosphonyl chloride 1 HNMR (400MHz, CDCl 3 ): δ4.56-4.51(m, 4H).

[0058] 19 F NMR (376MHz, CDCl 3 ): δ-74.2 (6F, J=8.6Hz, t).

[0059] GC-MS m / z (EI, 70ev): 281[M+1] + .

[0060] IR (thin film, cm -1 ): 1458, 1420, 1300, 1175, 1080, 970, 890, 848.

Embodiment 3

[0062] CH 2 Cl 2 (30mL) solution was added dropwise to CH 2 Cl 2 (20mL) solution, after the dropwise addition, keep at 0°C for 3h, rise to room temperature for 12h, add ethyl acetate to dilute and extract the reaction, wash the reaction solution with an appropriate amount of water to remove unreacted hydroxyethylacrylamide and The triethylamine hydrochloride that generates is washed with an appropriate amount of saturated aqueous sodium chloride solution, dried over magnesium sulfate, filtered, and spin-dried to obtain the acrylamide monomer (7.1g , yield 81%).

[0063] 1 HNMR (400MHz, CDCl 3 ): δ3.65-3.69 (m, 2H), 4.25-4.31 (m, 2H), 4.39-4.48 (m, 4H), 5.70 (dd, J=1.6Hz, 10.4Hz, 1H), 6.19 (dd, J=10.4Hz, 17.4Hz, 1H), 6.32(dd, J=1.6Hz, 17.4Hz, 1H), 6.88(s, 1H).

[0064] 19 F NMR (376MHz, CDCl 3 ): δ75.62 (t, J=8.65Hz, 6F)

[0065] GC-MS m / z (EI, 70ev): 345 [M-CH 2 ] + , 324[M-CH 2 -F] + , 305[M-C 3 h 3 O] + ,

[0066] 275[M-CH 2 -CF 3 ] + , 245[M-CH 2 -OCH ...

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Abstract

The invention relates to an acrylamide copolymer containing halothane and phosphoric acid ester as well as a preparation method and the application thereof. The preparation method comprises the steps of: (1) dissolving monomer, crosslinking monomer and non-fluoro long-chain monomer of the acrylamide copolymer containing halothane and phosphoric acid ester and emulsifier in deionized water and solvent for ultrasonically pre-emulsifying for 1-5h to obtain milk-white pre-emulsion; (2) under the protection of N2, heating 1/3 of the pre-emulsion to 60-90 DEG C, slowly dropping an initiator aqueous solution for initiating reaction, stopping dropping after the emulsion has blue fluorescence, combining the residual initiator aqueous solution with the pre-emulsion, slowing dropping the combined residual initiator aqueous solution and pre-emulsion into reaction liquid, stopping reaction after continuously reacting for 1-5h at 60-90 DEG C, and cooling down to the room temperature to obtain the required emulsion PFPA (Per Fluoro Propionic Anhydride). In the invention, cotton fabric processed by the copolymer emulsion has excellent performances of resisting water, oil and flame, the processing process is simple, and greater development potency is provided.

Description

technical field [0001] The invention belongs to the field of preparation and application of multifunctional finishing aids for fabrics, and in particular relates to a preparation method and application of an acrylamide copolymer containing fluoroalkyl phosphonate groups. Background technique [0002] At present, a lot of attempts have been made in the water and oil repellent finishing of fabrics. Fluorine-containing acrylate polymers contain perfluoroalkyl groups on the side chains, and the perfluoroalkyl side chains are oriented outwards, so their surface free energy is low, and they have good water and oil repellency, while acrylates have high The molecule itself has the characteristics of good film-forming property and relatively loose network structure, so the fabric treated with fluorine-containing acrylate fabric finishing agent can obtain excellent waterproof, oil-proof, anti-fouling, breathable, moisture-permeable characteristics and good chemical stability , therma...

Claims

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Application Information

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IPC IPC(8): C08F220/58C08F2/24D06M15/295D06M101/06
Inventor 孟卫东胡立立
Owner DONGHUA UNIV
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