JPS5846182A - Wash-and-wear processing treatment of cellulose fiber - 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 The present invention relates to a method of imparting wash-and-wear properties to a fibrous structure.

Conventionally, thermosetting resins such as urea/formaldehyde resins, melamine formaldehyde resins, and cyclic urea type resins, in other words, crosslinking agents, have been used to crosslink cellulose-based fiber structures to improve wash-and-wear properties (W&W properties). )
Many methods are known for imparting ease of care and ease of care.

To give an example, a cellulose-based fiber structure is immersed in an aqueous solution containing a cross-linking agent and a catalyst, and then squeezed with a squeezing roll so that the amount of cross-linking agent and catalyst attached is uniform. The most common method is the pad-dish-key method, which imparts WAW properties by drying and then heating at a constant temperature condition to cross-link the cellulose fibers with a cross-linking agent to improve rust-proof properties. It is well known and has been put into practical use. However, this method was insufficiently effective and did not fully satisfy WAW properties.

In order to further improve WAW properties. It is important to improve the wet wrinkle resistance as well as the dry wrinkle resistance.
It has been reported that good results can be obtained by applying a crosslinking agent uniformly within the fiber to effectively cause intermolecular covalent crosslinking. However, various methods are being investigated to control the crosslinking distribution.

Namely, there is a steam cure method in which heat treatment is carried out in a superheated steam atmosphere, a patch-up method called a moist cure method in which the condensation and reaction of resin is promoted in cotton fibers that contain several centimeters of moisture, and a moist cure method in which cotton fabric has a moisture content of 40%. % or more.Furthermore, in order to improve both dry and wet wrinkle resistance, wet crosslinking treatment is performed to impart moisture wrinkle resistance, and then para-cure, A 12-step treatment method that performs a dry crosslinking process consisting of dry and curing steps, or a dry crosslinking process after mercerization using liquid ammonia.
There are known methods for doing this. 'However, these conventionally known methods do not provide sufficient WA.
In order to obtain W properties, the processing time is extremely long, the process is complicated, the fiber strength deteriorates due to the use of harsh catalysts, and the processing equipment is corroded due to the influence of the catalyst. Various problems remain in putting it into practical use, such as the need for special processing equipment.

The present invention was devised in order to solve these problems, and uses a simple processing device to provide cellulose fibers with sufficient W&W properties through a simple and easy process without impairing the fiber properties. This is what we are trying to provide to the fabric.

The present invention will be explained in detail below.

The present invention consists of 1. After uniformly applying an aqueous solution containing a crosslinking agent and a catalyst to a cellulosic fiber structure, pre-drying is performed at 100° C. for 30 to 60 seconds. Then io'o℃~1
After steaming at a temperature of 30°C for 20 seconds to 5 minutes, immediately heat treatment at a temperature of 60°C to 140°C for 10 seconds to 6 minutes.
Heat treatment is performed for 0 seconds (hereinafter referred to as pre-heating), and then continuously heated at a temperature of 150°C to 200°C for 60 seconds to 1
This is a W&W processing method for cellulose fiber fabric, which is characterized by performing a heat treatment for 80 seconds (hereinafter referred to as post-heating).

That is, the present invention uses a wrinkle-proofing and cross-linking agent for ordinary Ω cellulose fibers that is generally used at present, and provides extremely excellent tower-proofing properties and W&W properties simply by devising the steaming treatment process and the subsequent heat treatment method. It is a simple, quick and inexpensive way to process cellulose fiber structures and products.

To explain the present invention in more detail using a cellulose fiber structure as a fabric, an ordinary powder mangling device or the like may be used as a method for applying an aqueous solution containing a crosslinking agent and a catalyst to a cellulose fiber fabric. It is not particularly limited to this, as long as it can be processed uniformly.

The cellulose fiber fabric containing the crosslinking agent, catalyst and water is then pre-dried. In this case, it is sufficient to simply dry the moisture contained in the fabric, and it is sufficient to dry it at 100° C. for 30 seconds to 60 seconds. - After that, steaming treatment is performed under a temperature condition of 100°C to 130°C.

The steaming treatment in the present invention has the effect of swelling the cellulose fibers, uniformly distributing the crosslinking agent within the fibers, and preventing localization of the crosslinking agent only on the fiber surface. In this case, the steaming treatment may be performed using saturated steam or superheated steam, but
In particular, steaming treatment using saturated steam at 100°C is suitable.

In this way, the treated fabric is immediately heated to 60°C to 140°C.
Preliminary heat treatment is performed at a temperature of ℃. Infrared heating or microwave heating is particularly suitable for this method.

As is well known, infrared heating, microwave heating,
Since internal heating is possible and has the effect of preventing localization of the crosslinking agent, by performing the preliminary heating with such a heat source, the crosslinking agent can be maintained evenly distributed within the fiber. However, the subsequent heat treatment may be performed continuously. Following the initial heating, the subsequent heating treatment is performed continuously at a temperature of 150°C to 200°C, so that the crosslinking agent evenly distributed within the fibers reacts with the cellulose molecules, resulting in good wrinkle resistance both when dry and when wet. In addition, it is possible to obtain a treated fabric with excellent easy-care properties, and also to prevent hardening of the texture and decrease in strength.

In addition, the effect of steaming treatment is more than simply distributing the crosslinking agent uniformly within the fiber through pre-heating, but by performing the steaming treatment beforehand, it improves the uniformity of the crosslinking agent within the fiber and the distribution of the crosslinking agent on the fiber surface. It is possible to further enhance the effects, such as preventing the localization of

Furthermore, even if ordinary heat treatment is used instead of infrared rays or microwave heating as the first stage heating method, the effect will be slightly inferior, but good results can of course be obtained by performing the first stage heating and the second stage heating continuously.

Appropriate pre-heating prevents the cross-linking agent uniformly distributed within the fibers from becoming localized and maintains a uniform distribution of the cross-linking agent, while the post-heat treatment continuously brings the cross-linking agent and cellulose fibers together. It works extremely effectively as preheating for the reaction.

Here, as an essential condition of the present invention, it is essential that the first-stage heating and the second-stage heating be performed continuously. Further, the post-heating method may be a commonly used hot air heating method.

The cellulose fiber structure described in the present invention includes powdered cotton,
Examples include cellulose yarn fibers such as hemp, polynosic, viscose, ammonium rayon, and mixed knitted fabrics and nonwoven fabrics of these and other synthetic fibers.

However, the crosslinking agents mentioned in the present invention are not limited to these, but specifically include the following. That is, dimethyloluron, dimethylolpropylene urea, dimethyloldihydroxyethyleneurea, dimethyloluron, trimethylolmelamine, trimethoxymethylmelamine, dimethylolmethyltriazone,
Dimethylol methyl triazone, dimethylol hydroxyethyl triazone, dimethylol methyl canibamate, dimethylol ethyl carbamate, dimethylol hydroxyethyl carbamate, etc. can be used.
Particularly preferably, N,N'-dimethyloldihydroxyethylene urea7. N,N'-dimethylolmonomethylolhydroxyethyleneurea, N,N'-methylol・
Methoxymethyl dihydroxyethyleneurea, N, N
Good results are obtained with '-methylethoxymethyl dihydroxyethyleneurea.

Specifically, the catalysts mentioned in the present invention include organic acids such as acetic acid and maleic acid, ammonium salts such as ammonium chloride and ammonium sulfate, amines such as ethanolamine hydrochloride, 2-amino-2methylpropanol hydrochloride, and magnesium chloride. Metal salts such as , nitric acid, zinc, zinc chloride, magnesium nitrate, zinc borofluoride, aluminum chloride, and magnesium phosphate can be used, and among these, magnesium chloride is particularly suitable in terms of effectiveness, workability, cost, etc.

Further, in the present invention, by adding a softening agent such as a higher fatty acid derivative or a silicone resin at the same time as a crosslinking agent and a catalyst, it is also possible to improve the texture, repellency, etc.

The process of the processing method of the present invention will be explained with reference to FIG. 1 of the drawings.
The sample is then immersed in a processing agent treatment bath (2) containing a crosslinking agent, a catalyst and, if necessary, a softener. Thereafter, it is squeezed with a squeezing roll (3), dried with a dryer (4), and introduced into a steamer (5) via a lead roll (R2). Thereafter, it is introduced into an infrared drying oven (6) via a lead roll (R3). Here, the infrared heater (pre-heated by force) is continuously introduced into the dry heat open (8) installed adjacent to the infrared drying oven (6). The fabric is washed with a saw pink bathtub via a lead roll (R4), washed with water in a water washing bathtub (10), and dried with an old dryer to obtain a processed fabric (121).

Figure 2 shows the case of microwave heating, which has a microwave heating furnace (I5) instead of an infrared drying furnace, and along with this, a filter (+3!Q4), a motor ( 16), a mode stirrer (17), and a microwave oscillator (181).

Hereinafter, the present invention will be explained in more detail using examples.

<Example-1> This example was carried out using the apparatus shown in FIG.

(1) A mercerized 100% cotton plain woven cloth (basis weight 989/d) was immersed in the following treatment solution (A) for ζ seconds, and then squeezed with a squeezing roll to achieve a squeezing rate of 80%. .

(a) Sumitex Resin NS-19 10 parts by weight (Crosslinking agent mainly composed of N, N' dimethylol dihydroxyethylene urea manufactured by Sumitomo Chemical Co., Ltd.) Magnesium chloride (filtrate salt) 35% aqueous solution 6i parts by weight Water 87
Total: 100 parts by weight (2) Next, this treated cloth was dried in an oven at 100°C for 40 seconds, and then this treated cloth was steamed for 3 minutes in normal pressure saturated steam at 100°C.

(3) Next, use four 1250W reflective infrared heaters, place the treated fabric at a position of 9CIn below the infrared heaters, heat it at 120℃ for 30 seconds, and immediately heat it to 160℃ without cooling. The resin was processed by heating continuously for 2 minutes in an open environment at ℃.

(4) Next, the obtained crosslinked cloth was washed in a washing bath at 40°C (
Household detergent Zab (Kao soap side) 2 'it/, I3
used) for 5 minutes, soaped, then washed with water and dried.

Resin-treated cloth (a) was obtained through these steps.

(5) Next, comparative samples were prepared using a commonly used resin processing method. (1) Treated cloth at 100℃, 40℃
Dry in the open for a few seconds, then dry the treated fabric at 160
℃ for 2 minutes in an open state to perform resin processing.

Next, this cross-linked cloth was soaped in a washing bath at 40° C. as in (4) to obtain a resin-treated cloth (BL).

(6) Next, the wrinkle resistance and WAW fiber strength of these (a) and (b) resin-treated fabrics and non-resin-treated fabrics were measured.

Comparing these measurement results, the results are as shown in Table 1 below.E Each evaluation was performed according to the following JIS standard.

Wrinkle resistance; JiS L-1096 (1979)
622 B method (sensant method) WAW property: // 623 B method (tumble drying method) Fiber strength; 〃 6.15.5. Method D (Pensulam method) (Table 1) From these results, the resin-treated cloth (a) shows good easy care and WAW properties, and is even better than the commonly used resin-treated cloth (b). A processed fabric with excellent easy care properties and W&Wi properties could be obtained.

<Example-2> This example was carried out using the apparatus shown in FIG.

(1) A mercerized 100% cotton plain woven cloth (basis weight 981/G) was immersed in the following treatment solution for 5 seconds, and then squeezed with a squeezing roll to achieve a squeezing rate of 80%. B) Sumitex Resin NS-1110 parts by weight (Crosslinking agent mainly composed of N, NL dimethylol monomethylol hydroxyethylene urea manufactured by Sumitomo Chemical Co., Ltd.) Magnesium chloride (filtrate salt) 35% water bath solution 3 parts by weight Water 87
〃Total 100〃 (2) Next, this treated cloth was placed in an oven at 100℃ for 40 seconds and dried. (3) Next, this treated cloth was introduced into a microwave continuous heating device equipped with an oscillator with a frequency of 2 a so' MII Z and an output of 2 KW, and microwave heating was performed for 20 seconds. (The surface temperature of the cloth was 97°C) 1 without cooling.
Resin processing was performed by continuously heating for 2 minutes in an open environment at 60°C.

(4) The obtained crosslinked cloth was soaped in a cleaning solution at 40° C. as in Example-1 to obtain a resin-treated cloth (q).

(5) Next, the treated fabric of (1) was dried in an oven at 100°C for 40 seconds, and then heated in an open oven at 160°C for 2 minutes to perform resin processing. Then Example-1
The resin-treated cloth (d) was obtained by soaping as follows.

(6) The wrinkle resistance, WAW properties, and fiber strength of these (C) and (d) resin-treated fabrics were measured as in Example-1. The measurement results are as shown in Table 2〇Table 2〉 Based on these results, the resin-treated cloth made of (C) has a wrinkle resistance degree, W
Good results were obtained in both the &W properties, and a practical resin-treated fabric with much better easy care and WAW properties than the treated fabric (d) was obtained.

<Example-3> (lj mercerized wood M 1.0'O% plain woven cloth (basis weight 98p/7rl'') was treated in advance with the following treatment solution (a) and treated in Example-1. The treatment was carried out as in (1).

(a) SUMITEX Resin NS-19 10]i parts bridging agent) Magnesium chloride (hexahydrate) 35% aqueous solution 3 parts SUMITEX SOFTNER L1.5// (Higher fatty acid derivative manufactured by Sumikata Chemical Co., Ltd.) System softener) water
85.5//total
100 parts by weight (2) Next, this treated fabric was dried as in Example-1-r21, and then steamed for 5 minutes in normal pressure saturated steam at 100°C. (3) (continuous heating was performed to obtain resin-treated cloth (e).

The results are shown in Table 6. These results show that by using a softener, (e) resin-treated cloth has better easy-care properties and W&F properties, and has better texture than (a) resin-treated cloth. I was able to obtain a good processed cloth.

l〈Example-4〉 (11 Silcare) Processed 100% cotton plain woven cloth (basis weight 98p/777”) was treated with the following treatment solution (A) in advance.
-(A) 10 parts by weight of Sumitex Resin NS-19 (manufactured by Sumitomo Kagaku Kogyo Co., Ltd., containing mainly N,N'-dimethyloldihydroxyethylene urea Crosslinking agent) Ammonium chloride 35% aqueous solution 6 parts by weight water
87 l/total 100 parts by weight (2) Next, this treated cloth was pre-dried as in (2) of Example-1, and then steamed for 3 minutes in normal pressure saturated steam at 100°C. Thereafter, continuous heating was performed as in (3) of Example-1 to obtain a resin-treated cloth (f). The result is the fourth
Write it down in the table.

(Table 4) From these results, (f) resin-treated cloth was slightly less effective than (Al resin-treated cloth), but - film properties (
b) Good results compared to resin-treated cloth.

<Example-5> (1) A mercerized 100% cotton plain woven cloth (basis weight 98 f'/771) was treated in advance with the following treatment solution (a) according to (1) of Example-1. I processed it like this.

(a) Sumitex Resin NS-16 101 parts (manufactured by Sumima Kagaku Kogyo Co., Ltd., crosslinking agent mainly composed of N,N'-methylolethoxymethyl-dihydroxy and ethylene urea) Magnesium chloride 3 parts by weight Water
87 total 10
0 parts by weight (2) Next, this treated fabric was pre-dried as in (2) of Example 1, and then steamed for 6 minutes in normal pressure saturated steam at 100°C.

(3) Next, this treated cloth was heated as described in (3) of Example-1 at 120°C for 130 seconds under an infrared heater, and continuously heated for 2 minutes in an oven at 160°C without cooling. As in Example-1 (soaping and resin-treated cloth (g
) was obtained.

(4) Similarly, the treated fabric of (2) was heated in the microwave for 20 seconds as in (3) of Example-2, and then heated continuously for 2 minutes in an oven at 160°C without cooling, and then A resin-treated cloth (h) was obtained by soaping as in -1.

(5) Similarly, the treated cloth in (2) was introduced into an oven at 120°C for 30 seconds, and heated for 1 to 10 minutes without cooling.
It was heated continuously for 2 minutes in an oven at 60°C, and then soaped as in Example-1 to obtain a resin-treated cloth (t>).

(6) Similarly, a comparative sample was prepared using a treated cloth (No. 11) using a commonly used resin processing method. (The treated cloth (No. 11) was dried in an oven at 100°C for 40 seconds, After returning to room temperature.

The cloth was heated in an oven at 160° C. for 2 minutes to perform resin processing, and then soaped as in Example-1 to obtain resin-treated cloth 0).

The wrinkle resistance W, &W property, and fiber strength of the resin-treated fabrics (g) to (j) were measured as in Example 1. The results are shown in Table 5.

From these results, (1) resin-treated cloth is (g) (h)
The result was slightly inferior to that of the resin-treated layer. but,
(j) Better easy care and W&
It showed W nature.

<Example 6> (1) A mercerized 100% cotton plain woven cloth (basis weight 98't7m) was treated in advance as in Example 1 using the following treatment solution (A). .

-(A) Sumitex Resin NS-1910 parts by weight (manufactured by Sumima Kagaku Kogyo Co., Ltd., crosslinking agent mainly composed of N, ■-dimethylol dihydroxyethylene urea) 3 parts by weight of 65% aqueous solution of magnesium chloride (hexahydrate) water 87 〃
Total: 100 parts by weight (2) Next, use four 250W reflective infrared heaters to place the treated fabric at a position of 9 CrrL below the infrared rays, heat it at 120°C for 60 seconds, and cool it. Immediately, the resin was processed by heating continuously for 2 minutes in an oven at 160°C.

(3) The resulting crosslinked cloth was then soaped in a cleaning solution at 40° C. as in Example 1 to obtain a resin-treated cloth (k).

(4) The wrinkle resistance, W&W properties, and fiber strength of this resin-treated cloth (k) were measured as in Example-1.

(k) Resin-treated cloth had a slightly stronger result than (a+m) resin-treated cloth, but showed better results than (b) resin-treated cloth. Therefore, the effect of steam treatment is It turned out to be big.

[Brief explanation of the drawing]

The drawings show embodiments of the present invention, and FIGS. 1 and 2 are explanatory diagrams of the apparatus used. (1)... Raw fabric (2)... Processing agent treatment tank (3)
... Squeezing roll (4) ... Dryer (5) ...
・Steamer (6)...Infrared drying furnace (7)...Infrared heater (8)...Dry heat open (9)...
Soaping bathtub (lO)...Washing bathtub α1)...
・Dryer 0...processed cloth (13+041...
Filter (1ω...Microwave furnace (16)
...Every time 07)...Mode stirrer patent applicant Toppan Printing Co., Ltd.

Claims (6)

[Claims] (1) After uniformly applying the crosslinking agent and catalyst to the cellulose fiber structure, steaming treatment is performed, and
Heat treatment (first stage heating) is performed for 10 seconds to 60 seconds at a temperature of 50 °C to 2.0 °C, and then continuously heated to 50 °C to 2.0 °C.
A wash and wear (W&W) processing method for cellulose fibers, which is characterized by performing heat treatment (post-stage heating) at a temperature of 6°C to 180 seconds. (2) The method described in claim 11, wherein the pre-heat treatment method is an infrared irradiation heating method. (3) The method described in claim 11, wherein the first stage heat treatment method is a microwave heating method. (4) The crosslinking agent is N,N'-dimethyloldi-1-droxyethyleneurea, N,N'-dimethylolmonomethyloxyethyleneurea, N,N'-methylolmethoxymethyldihydroxyethyleneurea, N %N'-
The method according to any one of claims (1) to (3), characterized in that one of methylolethoxymethyldihydroxyethyleneurea or a mixture thereof is used. (5) The method according to any one of claims 11 to 4, wherein the catalyst is magnesium chloride. (6) The method according to any one of claims (1) to (5), characterized in that a softening agent consisting of a higher fatty acid derivative and a silicone resin is applied simultaneously with the crosslinking agent and the catalyst. .