JPH06166952A - Scouring of woven fabric containing glass fiber - Google Patents

Abstract

PURPOSE:To provide a rational scouring method to enable the complete scouring of a woven fabric containing glass fiber at a low energy. CONSTITUTION:A woven fabric containing glass fiber is treated with low- temperature oxygen plasma, impregnated with an enzyme or a peroxide and washed after wet-heat treatment.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for scouring a fabric containing glass fibers.

[0002]

2. Description of the Related Art Fabrics containing glass fibers are often used for FRP and electronic print substrates, and are highly advanced in order to have sufficient adhesive strength between glass fibers and resin when they are impregnated with resin and laminated. Scouring process is required.

The conventional scouring process for glass fiber fabric is 30
Generally, a heat cleaning method in which an adhesive or an oiling agent is incinerated in an oven at a temperature of 0 ° C. or higher, or a method in which an enzyme such as amylase, a peroxide, and caustic soda are wet-processed to be scoured. In the case of a mixed woven product of glass fiber and thermoplastic fiber, scouring is performed only by a wet method.

Further, Japanese Patent Application Laid-Open No. 4-50359 proposes a method of heat-cleaning after scouring to some extent by a wet method.

[0005]

In the heat cleaning method, incineration must be performed in an oven at a high temperature of 300 ° C. or higher for several tens of hours or longer, and the degree of scouring is good, but energy and time are also required. Was also inefficient.

Although the wet method is efficient in terms of energy, it is difficult to completely remove the sizing agent and the oiling agent, and it tends to take time to raise the degree of scouring. Is dramatically increased.

In the method of Japanese Patent Laid-Open No. 4-50359, which combines a wet method and heat cleaning, heat cleaning is performed after scouring to some extent by the wet method, so that time efficiency and scouring degree are improved, but a high temperature of 300 ° C. or higher is used. It's not very energy efficient because things don't change.

Further, a scouring method incorporating heat cleaning into the process is possible in the case of a woven fabric consisting of only glass fibers, but it is not possible in a woven fabric composed of only thermoplastic fibers because the thermoplastic fibers are also incinerated. is there.

The present invention has been made in view of the above circumstances, and an object thereof is to obtain a method for reasonably refining a woven fabric containing glass fibers.

[0010]

The present invention achieves the above object and has the following structure. That is, according to the present invention, a woven fabric containing glass fibers is treated with a low temperature plasma of a gas containing oxygen, and then the woven fabric is impregnated with an aqueous solution of an enzyme or a peroxide, and then heat-treated at room temperature, or at room temperature for 10 hours or more. The gist is a method for refining a woven fabric containing glass fibers, which is characterized by allowing it to stand and then washing it. Hereinafter, the present invention will be described in detail.

In the method of the present invention, first, a woven fabric containing glass fibers is treated with a low temperature plasma of a gas containing oxygen. The term "woven fabric containing glass fibers" as used herein refers to a woven fabric made of only glass fibers used as warps or wefts, as well as a woven fabric that uses glass fibers only as warps or wefts, or one of warps or wefts. Or, it means a woven fabric or the like in which glass fibers are used every few fibers and the rest are composed of thermoplastic synthetic fibers. Here, the thermoplastic synthetic fiber is an ordinary thermoplastic synthetic fiber such as polyester, polyamide, polyacrylonitrile, polyether, vinylon, polyethylene, polypropylene, etc., and is appropriately selected according to the purpose of use.

In the method of the present invention, the above-mentioned woven fabric containing glass fibers is treated with low temperature plasma. Here, low temperature plasma means glow discharge in a mixed gas containing oxygen molecules such as oxygen gas or air under low pressure. Is caused by awakening,
It is a nonequilibrium plasma in which gas molecules are ionized and are in an excited and activated state.

First, the inside of a vacuum pressure-resistant container containing a woven fabric containing glass fibers is evacuated to a pressure of 0.1 torr or less by a vacuum pump, and then a mixed gas containing oxygen molecules such as oxygen gas and air is introduced to reduce the pressure to 0. Adjust the gas concentration within the range of 1 to 2.0 torr. If it is 2.0 torr or more, glow discharge becomes difficult to occur, and a sufficient low temperature plasma treatment effect cannot be applied to the glass fabric. Next, electric energy is applied to the electrodes inside the vacuum container to cause glow discharge. The electric energy source may be either a DC voltage application or an AC voltage application, but it is preferable to apply a high frequency AC voltage of 1 KHz to 3000 MHz in terms of energy efficiency.

The treatment time of the glass fiber-containing fabric by the low-temperature plasma varies depending on the shape, thickness, and weight of the glass fiber-containing fabric, but it is usually 30 to 90 seconds when it is kept in the low-temperature plasma state. The effect is obtained.

After the low temperature plasma treatment, in the method of the present invention, the woven fabric containing glass fibers is impregnated with an aqueous solution of an enzyme or a peroxide, subjected to wet heat treatment, and then washed. Examples of the enzyme include α-amylase and β-amylase, and examples of the peroxide include sodium bromate, potassium peroxodisulfate, ammonium peroxodisulfate, and the like.

The wet heat treatment may be carried out using a steamer, open soaper, jigger, etc.
You must be careful not to break or rub it. This is because if the glass fiber is significantly damaged, the quality will deteriorate when processed into an FRP or electronic printed circuit board. The wet heat treatment is usually performed at 60 to 120 ° C. for 0.5 to 60 minutes. When removing the sizing agent using an enzyme, a so-called cold batch method in which the enzyme solution is impregnated and then left at room temperature for several tens of hours can be used in addition to the wet heat treatment.

After the above-described low temperature plasma treatment, the oiling agent may be removed by washing with a surfactant. The washing with the surfactant may be performed before or after desizing, and from the viewpoint of streamlining the process, a method of impregnating the fabric at the same time with the desizing agent and subjecting it to wet heat treatment can be used.
The degree of scouring becomes a little worse. After removing the sizing agent and oiling agent, wash thoroughly with pure water and dry. When a woven fabric containing glass fibers is used for an electronic printed circuit board in particular, if metal ions such as sodium remain, the insulating property deteriorates and the quality deteriorates.

[0018]

[Operation] When a fabric containing glass fibers is treated with a low-temperature plasma of a gas containing oxygen, the sizing agent and oiling agent attached to the fiber surface chemically breaks the molecules, resulting in a rapid dissolution rate in water. In addition, hydrophobic substances such as oiling agents have oxygen atoms introduced into the molecule and hydrophilic groups such as carboxyl groups and hydroxyl groups are generated on the surface, greatly improving the wettability of the fiber surface. The formation of these hydrophilic groups improves the water absorption and the water solubility.
If the fiber is scoured in such a state, the scouring can be performed very efficiently.

[0019]

EXAMPLES Next, the method of the present invention will be described in more detail with reference to Examples.
The procedure was as follows. (1) Ignition loss rate According to JISR-3420, the weight loss rate of the sample after scouring was measured. (2) Residual carbon amount SUMIGRAPH NC-80 manufactured by Sumitomo Chemical was used to measure the residual carbon amount.

Example 1 44 warps / inch, 33 wefts / inch of a glass fiber having a fineness of 68 tex, a thickness of 180 μm, and a basis weight of 21
A glass fiber fabric of 0 g / m ² was subjected to a low temperature plasma treatment for 60 seconds by applying a high frequency voltage of 13.56 MHz in frequency and 1.5 W / cm ² in output under a pressure of 1 torr of oxygen gas.

Next, a 0.2% aqueous solution of Biotex TS (heat-resistant amylase, manufactured by Nagase Biochemical Co., Ltd.) was impregnated at a pickup rate of 60%, steamed at 104 ° C. for 30 seconds, and then Neugen SS (Nonion). Surfactant,
30% in a 0.5% aqueous solution of Daiichi Kogyo Seiyaku Co., Ltd.)
It was washed for 2 seconds, finally washed thoroughly with pure water and dried with an infrared dryer.

For comparison with the method of the present invention, a scoured woven fabric for comparison (Comparative Example 1) was prepared in the same manner as in this Example except that the low temperature plasma treatment step was omitted in this Example.
Got

The performances of the inventive and comparative fabrics were measured and the results are shown in Table 1.

[0024]

[Table 1]

As is clear from Table 1, the scoured woven fabric produced by the method of the present invention has a low ignition loss rate and a small amount of residual carbon, and is satisfactorily scoured.

Example 2 In Example 1 described above, the 0.5% aqueous solution of Biotex TS (heat resistant amylase, product of Nagase Biochemical Co., Ltd.) was replaced with Biotex SL (persulfate) manufactured by the same company. A scoured fabric of the present invention was obtained in the same manner as in Example 1 except that a 1.0% aqueous solution was used.

For comparison with the method of the present invention, a scouring woven fabric for comparison (Comparative Example 2) was prepared in the same manner as in this Example except that the low temperature plasma treatment step was omitted.
Got

The performances of the invention and comparative fabrics were measured and the results are shown in Table 2.

[0029]

[Table 2]

As is clear from Table 2, the scoured fabric produced by the method of the present invention has a small loss on ignition and a small amount of residual carbon, indicating that the scouring is carried out very well.

Example 3 First, a plain woven fabric (warp density: 44 yarns / inch, weft yarn: 33 yarns / inch) using glass fibers having a fineness of 68 tex and warp yarns of polyester filament 780d / 78f was prepared. After low-temperature plasma treatment under the same conditions as in Example 1, a 0.2% aqueous solution of Biotex LS (persulfate, a product of Nagase Biochemical Co., Ltd.) was picked up at a pick-up rate of 6
It was impregnated with 0%, batched up and left at room temperature for 16 hours. Next, it was washed for 30 seconds in a 0.5% aqueous solution of Neugen SS (nonionic surfactant, manufactured by Daiichi Kogyo Seiyaku Co., Ltd.), and finally, washed thoroughly with pure water and dried by an infrared dryer.

For comparison with the method of the present invention, a scoured woven fabric for comparison (Comparative Example 3) was prepared in the same manner as in this Example except that the low temperature plasma treatment step was omitted in this Example.
Got

The performances of the invention and comparative fabrics were measured and the results are shown in Table 3.

[0034]

[Table 3]

As is clear from Table 3, the scoured fabric produced by the method of the present invention has a small loss on ignition and a small amount of residual carbon, and is satisfactorily scoured.

[0036]

According to the method of the present invention, a woven fabric containing glass fibers can be reasonably completely scoured with a small amount of energy.

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Claims (1)

[Claims] 1. A woven fabric containing glass fibers is treated with a low temperature plasma of a gas containing oxygen, and then the woven fabric is impregnated with an aqueous solution of an enzyme or a peroxide, followed by heat treatment for moistening, or at room temperature for 10 hours. A method for scouring a woven fabric containing glass fibers, which comprises leaving the above for a while, and then washing it.