WO2015099520A1

WO2015099520A1 - Grafting of ionic liquids onto textile materials by a sol/gel method for the development of special-purpose fabrics

Info

Publication number: WO2015099520A1
Application number: PCT/MA2014/000056
Authority: WO
Original assignee: Ecole Superieure Des Industries De Textile Et De L'habillement; Centre National Pour La Recherche Scientifique Et Technique; UNIVERSITE HASSAN II de CASABLANCA
Priority date: 2013-12-18
Filing date: 2014-12-17
Publication date: 2015-07-02
Also published as: MA20150438A1; MA36586B1

Abstract

The invention relates to a method for the functionalisation of a textile in order to provide it with anti-bacterial, heat-resistance and/or anti-wettability properties. Said method comprises the following steps: formulation of a solution consisting of a water/alcohol mixture, salt derived from siloxysilane and an acid; impregnation of the textile in said solution; drying of the textile material in order to ensure the grafting of the substrate by reaction of the reactive groups; and anion exchange in order to provide the textile with the desired properties if necessary.

Description

Title: Grafting of ionic liquids onto textile materials by soil / gel for the development of dedicated tissue

Description:

The invention relates to a method of functionalizing a textile in order to confer antibacterial properties, heat resistance and / or antiwettability to said textile, as well as a functionalized textile by implementing such a method.

In particular, a textile thus functionalized can be used under conditions of exposure to heat, especially by heating, for example a protective clothing, work, military or automotive applications. According to other applications, the functionalized textile can be used for the production of anti-bacterial articles, in the form of articles made in blouses or combinations or in the form of wipes, nonwoven strips, etc.

The aim of the invention is to propose a method of functionalization which is simple to implement and able to give a textile optimum antibacterial properties, resistance to heat and / or anti-wettability, and this in a particularly reliable manner. For this purpose, according to a first aspect, the invention proposes a method of functionalizing a textile in order to give it antibacterial, heat-resistant and / or anti-wettable properties to said textile.

The method comprising the steps of:

Formulate a solution consisting of a mixture of water, alcohol, a siloxane salt and an acid;

Impregnate the textile in the said solution

Dry the textile material to ensure the grafting of the substrate by reaction of the reactive groups.

Exchange the anion in order to give the textile the desired properties if necessary.

According to a second aspect, the invention proposes a functionalized textile by implementing such a method, said textile comprising a material capable of imparting antibacterial properties, heat resistance and / or antiwettability to said textile.

Other features and advantages of the invention will appear in the description which follows, made with reference to the appended figures, in which:

FIG. 2 is an image recorded by a scanning electron microscope (SEM) of a functionalized textile according to one embodiment of the invention;

- Image is an image showing the anti-wetting properties of a functionalized textile by implementing a method according to the invention.

In relation to these figures, there is described below a textile A functionalized with a siloxane salt capable of giving it the desired properties, as well as a method of functionalizing such a textile A. In particular and as an example, the textile A may be a knit, a fabric, a nonwoven or another textile-originated substrate.

The functionalization steps are listed below:

Step 1: Prepare the solution:

The salts used to prepare the solution are synthesized according to the reaction scheme (schematic) from the precursor (3-chloropropyl) triethoxysilane and 1-methylimidazole or pyridine.

0.2 mol (1 equivalent) of 1-methylimidazole or pyridine and 0.2 mol (1 equivalent) of the CPTS ((3-chloropropyl) triethoxysilane) are placed in a flask surmounted by a condenser with stirring at 100 ^° C. in the case of methylimidazole and 115 ° C in the case of pyridine.

After 18 hours, an orange oil is obtained in the case of MCPTS and a brownish oil in the case of PCPTS which are then used without purification.

The structures of the salts obtained were confirmed by proton NMR, infrared spectroscopy to transform fourrier mass spectrometry.

The method provides for formulating a solution comprising a medium consisting of a mixture of water and ethanol; the salt derived from siloxane, and an acid as catalyst according to the following protocol:

In a flask surmounted by MCPTS / PCPTS refrigerant, distilled water, EtOH (99%) and HCl (37%) are mixed with MCPTS / HCl / EtOH / H2O, 5 / 0.008 / 60/55) with stirring. for 3 h at 70 ° C.

Step 2: The tissues are then emerged in the prepared soils for a determined time depending on the desired properties. The fabric is then padded until reaching a "pick-up" of 80

%

Step 3: The fabric is dried at 80 ° C for 1 h and then at 120 ° C for 1 h in an oven.

Diagram 2 illustrates the hydrolysis and condensation reactions involved during cotton functionalization by the sol gel route (Step 2 and 3)

Step 4: Metathesis step or anion exchange:

The coated textile is impregnated in a dilute solution of HPF6 (0.66 mol / l) (scheme 3) and then washed 3 times with distilled water and dried at 80 ° C. at 120 ° C. overnight.

Characterization of functionalized tissues.

Infrared Spectroscopy: 1083cm-1 (v, Si-C), 842 cm-1 (v, PF6 -) (FIG. 1)

SEM scanning electron microscopy analysis:

Figure 2 illustrates SEM images of the front cotton (Figure 2-a) and after the reaction of metathesis (Figure 2-b). Figure 2-b shows the formation of a film on the surface of the cotton fiber. The The microanalysis by EDX of the PF6-functionalized textile shows the presence of N, P, F, Si, which allows us to conclude that the grafting was well done. (See Figure 3)

Properties of non-wetting, antibacterial activity and thermal stability of functionalized tissues.

Non-wettability test

a- Test of the drop of water:

Using a capillary we deposited a few drops of colored water on both the treated and untreated textiles. As shown in Figure 1, the tast of colored water was adsorbed by the non-cotton fabric. treated (see (picture A)). On the other hand, the drops remain on the surface of the fabric functionalized by PF6 (see, image B). b- adsorption test of treated textiles:

The water adsorption test consists in depositing the prepared samples of (5cmx5cm) in 150ml of distilled water for 1min.

Figure 4 illustrates the variation of the adsorption rate for each fabric as a function of the drying temperature.

In the case of MCPTS-treated cotton, As illustrated in Figure 4-a the adsorption rate was reduced by 340% for the 235% untreated sample and 51% for the dried sample after metathesis for 120%. ° C and 80 ° C respectively. Similarly, in the case of PCPTS treated cotton, As illustrated in Figure 4-b, the adsorption rate was reduced by 340% for the untreated sample at 240% and 48% for the dried sample after metathesis during 120 ° C and 80 ° C respectively.

Thermal stability of treated fabrics:

Figure 5 illustrates thermogravimetric curves of uncoated and PF6-coated fabrics via MCPTS.

In the case of uncoated cotton, the degradation has three main stages. The first stage starts at 354 ° C and involves two competitive pathways which are the release of volatiles and carbonization of the aliphatic products. The second stage starts at 487 ° C., which corresponds to the conversion of the carbonated aliphatic products to the aromatics producing the mono and carbon dioxide. The third stage starts at 800 ° C. and corresponds to the oxidation of the carbonized products. In the case of coated cotton, the degradation has several stages. The first step ends at 287 ° C in which the rate of decomposition is very fast. During the second and the last step the rate of decomposition slowly decreases until the dehydration and carbonization of the fiber at 900 ° C. Unlike the untreated sample which was decomposed in two stages with a very fast rate of degradation. For comparison the weight loss at 900 ° C was 90% for the PF6 sample while it was 99% for the untreated sample. (Table 1)

Claims

A method of functionalizing a textile (1) to impart antibacterial properties, anti-wettability and / or heat resistance, said method comprising:

Formulate a solution consisting of a mixture of water / alcohol, salt derived from siloxysilane and an acid. Impregnate the textile in the said solution

Exchange Panion in order to give the textile the desired properties.

2. Method according to claim 1, characterized in that the solution comprises between 1 and 50 mol of alkyltrialkoxysiloxane salt, dialkyldialkoxysiloxane. The alkyl group may consist of a C3 to C40 carbon chain.

3. Method according to claim 2, characterized in that the solution comprises 55 mol and 60 mol of alcohol.

4. Method according to claim 3, characterized in that the solution comprises between 0.008 and 1% of hydracid.

5. Method according to any one of claims 1 to 4, characterized in that the film is deposited by impregnation of the fabric, fiber or file.

6. Method according to any one of claims 1 to 5, characterized in that the drying is carried out in two stages.

7. Method according to any one of claims 1 to 6, characterized in that the anion exchange is by impregnation of the textile in a salt solution or anionic acid between 1 to 10 mol%.

8. Process according to claim 1 to 7, characterized in that the anion can be chosen from anion derived from phosphate, sulphate, triflimide, halide, fulroborate, fluorophosphate, acetate, etc.

9. Textile functionalized by carrying out a method according to any one of claims 1 to 8, said textile comprising a film capable of imparting antibacterial properties, heat resistance and / or antiwettability to said textile.