JPS6170080A - Production of durable water repellent cloth - Google Patents

Abstract

(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application of the Invention] The present invention relates to a method for producing a durable water-repellent fabric.

[Prior Art] In recent years, there has been an increasing demand for water repellency mainly in the field of sports clothing, and with this, there is a strong desire to improve the durability of water repellency against dry cleaning, washing, etc.

Currently, fabrics are made water repellent by treating them with silicone or fluorine-based water repellents.

However, silicone-based water repellents easily swell with dry cleaning solvents such as trichlene and percrene.
Because it dissolves, it has almost no durability against dry cleaning, and silicone alone has a low level of water repellency, so it currently cannot meet the advanced demands of recent years.

On the other hand, fluorine-based water repellents have a high initial level of water repellency, but the resin coating is hard and brittle, so they have the disadvantage that the resin coating can crack when washed or rubbed during wear, resulting in a decrease in water repellency. , all of which are A2 i (not updated) in response to recent advanced requirements.

In addition, when water-polished products made of conventional silicone or fluororesin undergo washing or dry cleaning processes, the main chains of polymers that have a strong affinity with washing solution W, especially water, form a resin coating. This had a serious drawback in that the methyl groups or -CFsWi, which tend to appear on the surface and are involved in water repellency, penetrate into the control coating, resulting in a significant drop in water repellency.

On the other hand, as proposed in Japanese Patent Application No. 57-187776 (!i!), applying silicone compounds to fibers and then subjecting them to low-temperature plasma treatment improves the color depth of dyed products and increases their durability. However, it is obvious that this fabric is not suitable for the purpose of the present invention because hydrophilic groups are introduced to the surface of the fabric and it becomes hydrophilic by plasma treatment. .

Therefore, the present inventors conducted various studies on a method for obtaining a water-repellent fabric that has high water-repellent performance and excellent durability against washing or dry cleaning, and developed the present invention.

That is, the present invention has the following configuration.

[Structure of the Invention] A durable water-repellent fabric characterized by applying a treatment liquid of an organopolysiloxane, a fluorine-containing compound, or a mixture thereof, followed by low-temperature plasma treatment, and then heat treatment at a temperature of 70°C or higher. Made and transmitted.

[Means for Solving the Problem] Here, the organopolysiloxane compound and 1 can be used by suitably preparing 11R of a silicone-based 1g solution that is generally used as an old solution or a softener. Examples include oils or emulsions of dimedylbolysiloxane and polysiloxane compounds modified by introducing hydroxyl groups, amine groups, hydrogen, epoxy groups, polyether groups, etc. into the terminals or side chains of dimethylpolysiloxane molecules. .

In addition, fluorine-containing compounds are usually polyallylic acid esters made of polyacrylic acid and fluorinated alcohol, for example,
Examples include polybentadecaf J rheoloocdyl acrylate, polytrifluoroethyl acrylate, polytrifluoroethyl methacrylate, and fluorine-based hydrocarbons such as tetrafluoroethylene-hexafluoropropylene copolymer.

After applying these 18 liquid agents to the fabric, the steps of subjecting it to low-temperature plasma treatment and heat treatment at 70° C. or higher are essential steps of the present invention.

In other words, it is known that the resin coating surface is cross-linked and insolubilized by low-temperature plasma treatment, but if a fabric coated with the above mixture is simply subjected to low-temperature plasma treatment, its water repellency will actually decrease and it will most likely become hydrophilic. However, the object of the present invention cannot be obtained. but,
Excellent water repellency is achieved by heat-treating this at a temperature of 70°C or higher to regenerate the methyl groups or -CF3 bases involved in water repellency from under the crosslinked film formed on the resin film surface. The present invention is characterized by its durability.

That is, the resin coating is
? ! In addition to improving its durability against washing and dry cleaning, the water-repellent surface regenerated by passing through a dense crosslinked film through heat treatment absorbs energy equivalent to the affinity of the cleaning solvent and the polymer main chain. In this case, the groups involved in water repellency are not buried in the resin, and the aqueous level of 1a immediately after treatment can be maintained.

The low-temperature plasma treatment referred to here involves exposing the object to be treated to plasma generated by a sustained discharge initiated by applying a high voltage, and there are various forms of such discharge such as corona discharge and glow discharge. There is, but U&
Although there are no particular limitations on the discharge form as long as it does not give a rough thermal loss (n), glow discharge is more preferable in order to obtain uniformity of treatment effect as well as uniformity of discharge.

The glow discharge mentioned above is a discharge that starts and continues when a high voltage is applied in a gas atmosphere under low pressure. Processing conditions such as discharge power, gas pressure, and processing time are determined by the type of resin, processing equipment, etc. The key point is that conditions can be selected that can crosslink (n) insolubilize the silicone resin on the fiber surface.

The gases used for this low-temperature plasma treatment are Am, N2゜He,
Commonly used gases such as CO2, CO2, CF4, air, and 7kM gas can be used, but in order to efficiently crosslink silicone resin, CO2°02, CF4.
It is preferable to avoid the use of gases with high etching ability, such as air, as much as possible.

In addition, the heat treatment that follows the low-temperature plasma treatment is
Develops water repellency that disappeared due to low-temperature plasma treatment,
This is essential in order to obtain a sustained ω water effect, but it requires a temperature at which sufficient thermal movement of polymer molecules occurs and a sufficient time for the surface of the fabric to be heated.
A heating time of several seconds or more is required at a temperature above, preferably 100° C. or above, depending on the thickness of the fabric, etc.

In addition, it is necessary to heat the entire fabric uniformly, and the most preferable method is to heat it in a hot air treatment field.
From the viewpoint of uniform processing, it is preferable to carry out the process before the product is sewn. Heating with an iron or the like after sewing only results in uneven treatment, which does not take away from the object of the present invention.

In addition, water repellent agents such as organopolysiloxane or fluorine-containing compounds are applied to fabrics in the form of a solvent solution or an emulsion dispersed with an emulsifier, etc., and then dried. Application of the treatment liquid can be performed using the pad method, dipping, etc. You can use commonly used methods such as
It can be selected depending on the purpose.

In addition, the fabric referred to in the present invention refers to an IT product made of natural fibers, recycled fibers, synthetic fibers, or a mixture of these fibers,
This refers to nonwoven fabrics, etc.

Hereinafter, the present invention will be explained in more detail based on Examples, but the present invention is not limited thereto.

Example 1 Nylon taffeta using 75 denier 36 filament nylon thread (width 120 cm, basis weight 103 g/m, density vertical/E: +” 130/100 (strands/inch))
After performing normal scouring and heat setting, the following water repellent treatment was performed to evaluate β aqueous property and its washing/dry cleaning durability.

Note that water repellency is measured by a test method (spray method) specified in JIS-L1079. Further, durability was determined by repeating the following washing or dry cleaning test 20 times, and then performing the above water repellency test.

For washing, use an automatic reversing whirlpool electric washing machine (Toshiba vH11)
Add 0.2% slightly alkaline synthetic detergent >Fi specified by LIIS K337 at 40°C ± 2°C to a washing machine (Model 50), add additional cloth so that the bath ratio is 1:50, and wash on strong conditions for 1Q. Then, the process of draining the water and washing with water for 5 minutes was repeated 20 times, and then air-dried.

For dry cleaning, use a dry cleaning cylinder (approximately 22 crta in diameter and 133 cm in length).
') > da,) 50 from the axis, tilt the axis, 845 ~ 5
3.8αε of perchlorethylene at room temperature was placed in a tube (rotating at 0 rpm), 230 g of test piece was placed therein, and the test piece was rotated for 10 minutes. This process was repeated 50 times, and then air-dried.

(Resin treatment liquid) A, Toray Silicone 5H-8240 (Both ends -〇H modified silicone emulsion, active ingredient 40%, manufactured by Toray Silicone Co., Ltd.) 30C)/α water dispersion B, Asahi Guard AG-710 (Fluorine-based old water agent, manufactured by Asahigarus Co., Ltd.) 40 Q/(l water i'll iWC, Toreshi') Corn, 5H-824015o/II Aqueous dispersion containing Asahi Guard AG-71015g/α.

The resin treatment was carried out by immersing the fabric in these treatment solutions, applying treatment ia of 35% based on the weight of the fabric using a mangle, and drying for 3 minutes in a hot air dryer at 130°C.

(Plasma treatment conditions) Gas/pressure argon 0.6 Torr applied voltage: 2
KV processing speed = 30cm/min Number of electrodes: 1 (dry heat treatment conditions) Hot air dryer ■ 70"CXS minutes ■ 100"CX 30 seconds The following table shows the results of examining the β-aqueous nature and its durability of these treated samples. Shown below.

(Note) The relationship between appearance condition and point allocation is as follows.

100 points 2. If the surface shows adhering moisture 90 points If the surface shows slight adhering moisture 80 points If the falling point of water on the surface shows wetting 70 points If the entire surface shows partial wetting 50 points Those showing moisture on the entire surface ○ Those showing complete moisture on the surface The only water Ql of the present invention showed good old water properties with a score of 90 or higher even after washing and dry cleaning. .

[Effect of the invention 1] The present invention eliminates washing'+M, which was a drawback of conventional processed products.
Alternatively, it is possible to provide a superior product that does not suffer from a decrease in 1,9 aqueous properties due to dry cleaning.

Claims (1)

[Claims] A method for producing a durable water-repellent fabric, which comprises applying an organopolysiloxane compound, a fluorine-containing compound, or a treatment solution containing a mixture thereof, followed by low-temperature plasma treatment, and then heat treatment at 70°C or higher.