JP3130148B2 - Method for preventing fibrillation of solvent-spun cellulosic fibers - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001] The present invention relates to a method for preventing fibrillation of a solvent-spun cellulosic fiber.

[0002] The "fibrillation" of fibers is a phenomenon in which fibers are physically split by washing or other actions.
It is a phenomenon different from so-called fluffing and pilling,
Fuzzing and pilling may occur as a result of fibrillation of the fibers.

[0003] Solvent-spun cellulosic fibers, for example, "TENCEL" (trade name) of Coatles Co., Ltd., have the outermost layer of the fiber that coagulates most quickly during the desolvation stage during spinning, due to physical friction and impact. When subjected to this, the bark is fibrillated so that the bark is peeled off, fuzzing or pilling is caused by washing or the like, and it cannot be used for applications of textile products such as clothing and bedding which are repeatedly washed.

[0004] The inventors of the present invention have intensively studied measures for preventing such fibrillation. As a result, when the cellulose fiber is treated with an N-methylolated amine compound, the fibrillation of the fiber is extremely effective. It has been found that the present invention can be prevented, and the present invention has been completed.

Thus, the present invention provides a method for preventing fibrillation of a solvent-spun cellulosic fiber, which comprises treating the solvent-spun cellulosic fiber with an N-methylolated amine compound. is there.

The "solvent-spun cellulosic fibers" to be treated in the method of the present invention include cellulose or pulp which can be dissolved in a solvent capable of dissolving them, for example, N-methylmorpholine-N-oxide, dimethyl sulfoxide, Fibers produced by spinning a solution dissolved in -methylpiperidine-N-oxide, dimethylacetamide, or the like by a dry or wet spinning method, and the one that is currently in practical use is N-methylmorpholine-N of pulp.
-Only "TENCEL" (trade name) manufactured by Courtes Ltd. UK spun from an oxide solution.

[0007] This Tencel has a very strong strength as compared with rayon, and has excellent characteristics such as being hard to shrink, but it also has the best properties of the fiber which coagulates most quickly at the stage of desolvation during spinning. When the outer layer is subjected to physical friction or impact, it has the disadvantage of causing fibrillation so that the bark is peeled off. Due to this drawback, it has been difficult to use it for clothing and bedding that has frequent washing while having other excellent characteristics.

The inventors have found that fibrillation of Tencel occurs only in the outermost layer of the fiber, and a method of removing a portion to be fibrillated, a method of coating the fiber with a resin so that the fiber is not fibrillated, Alternatively, a method of crosslinking between fibers was studied.

[0009] A method for removing a portion to be fibrillated by a cellulolytic enzyme is to impregnate a solution of cellulase, a cellulolytic enzyme, with a fabric of Tencel,
This is a method in which the cellulase is treated with a liquid dyeing machine or the like in the active temperature range. Although this method is effective in preventing fibrillation, it is inevitable that the fiber strength is reduced because cellulose is decomposed with an enzyme. Therefore, when trying to completely prevent fibrillation, the fiber strength is considerably reduced,
It is difficult to maintain practical strength.

On the other hand, processing with a resin is performed by using a film-forming polymer resin such as a polyacrylic resin, a polyurethane resin,
A method of coating the fiber with a polysilicon resin;
There are two methods of crosslinking between fibers using a methylolated amino resin, and in our experiments, a method of crosslinking between fibers has a much higher effect than a method of coating fibers with a resin. I found that I can do it.

The N-methylolated amine compound used for the crosslinking treatment of the solvent-spun cellulosic fiber may be a primary or secondary amino compound such as urea resin, urea glyoxal resin or melamine resin. Group (NH
_2- or -NH-) in which the amino group is methylolated in a compound containing at least two or more,
The methylol group may be further at least partially modified by alkoxylation, silylation and the like. Specific examples of such N-methylolated amine compounds include dimethylol urea, methylol melamine, dimethylol ethylene urea, dimethylol propylene urea, dimethylol dihydroxy ethylene urea, dimethoxy methylol dimethoxy ethylene urea, dimethylol dimethoxy ethylene urea, Examples include dimethyloluron, and among them, dimethyloldihydroxyethyleneurea is preferable.

The treatment of the cellulosic fibers with the N-methylolated amine compound is carried out, for example, by impregnating the cellulosic fibers with an aqueous solution containing the N-methylolated amine compound and a cross-linking catalyst, drying the fiber if necessary, 10
It can be carried out by heating to a temperature of 0 to about 200C, preferably about 120C to about 160C.

The concentration of the N-methylolated amine compound in the above aqueous solution is not strictly limited, and can be varied over a wide range depending on the type of the compound, but is generally 30 to 300 g / l. Preferably 60-1
A range of 50 g / l is expedient. Examples of the crosslinking catalyst include metal compounds such as magnesium chloride, zinc borofluoride, and aluminum oxide; and acids such as citric acid, phosphoric acid, and sulfuric acid. Their use amount can usually be in the range of 1 to 50 parts by weight, especially 5 to 35 parts by weight, per 100 parts by weight of the methylolated amine compound.

The impregnation amount of the aqueous solution of the N-methylolated amine compound is generally 50% owf to 120% owf,
Preferably, it can be in the range of 70% owf to 100% owf.

The cellulosic fiber is in a filament state,
It can be treated in any form such as a spun yarn, a woven or knitted fabric, or a non-woven fabric.

The treatment method of the present invention can be combined with an enzyme treatment. That is, the solvent-spun cellulosic fiber is preliminarily subjected to cellulase, for example, joint liquor refinement “Gordo TCL”, Nakuto Kasei “Enchilon CM”, Nagase Seikagaku “Cell riser”, Novo Nordisk sp35
9. After treatment with a cellulose-degrading enzyme such as "Meylase" manufactured by Meiji Seika, it can be treated with an N-methylolated amine compound according to the method of the present invention.

The treatment with an enzyme can be carried out by a method known per se. For example, an optimal p
The cellulosic fiber is immersed in an aqueous solution of the enzyme adjusted to H (about 4.5 to about 6.5), and activated temperature (optimum temperature; about 45 to about 6.5).
(About 60 ° C.).

As is apparent from the following examples, the cellulosic fibers treated by the method of the present invention do not fibrillate even in the subsequent repeated washing test, and for example, the repetition of underwear, wisdom, etc. It can be widely used in clothes to be washed and beddings such as sheets.

Next, the present invention will be described more specifically with reference to examples.

[0020]

EXAMPLES Example 1 As solvent-spun cellulosic fibers, Tencel (a fineness of 1.5 d, 38 mm) manufactured by Coatles Co., Ltd. was spun into a 40th yarn, and a 40 × 40/131 × 70 broad was woven.

The woven fabric was immersed in an aqueous solution having the formulation shown in Table 1 below, squeezed to 70% of pick-up with a mangle, dried, and baked at 160 ° C. for 2 minutes.

The treatment liquid used was a polyacrylic acid resin, a polysilicon resin, or a polyurethane resin which coats the fibers for comparison, in addition to the N-methylolated amine compound which crosslinks the fibers.

The obtained treated cloth was subjected to JIS L 1042 (F
Washing was repeated 10 times in accordance with (-2 method), and the degree of fibril was observed with an electron microscope. According to the invention, N
Formulation 1 treated with the methylolated amine compound showed little fibrillation, but Formulations 2 to 5 treated with other resins covering the fibers showed fibrillation. As a comparative example, untreated ones without resin processing also produced fibrils when similarly washed.
Fluffing and pilling occurred.

[0024]

[Table 1]

Example 2 Tencel (a fineness of 1.5 d, length of 38 mm) manufactured by Coatles Co., Ltd., which is a solvent-spun cellulose fiber, was spun into a 40-th yarn to produce a 40 × 40/131 × 70 plain woven fabric.

The woven fabric is dipped in aqueous solutions of various N-methylolated amine compounds having the formulations shown in Table 2 below, squeezed to 70% of pick-up with a mangle, dried, and baked at 160 ° C. for 2 minutes. Was.

The obtained treated cloth was subjected to JIS L 1042 (F
Washing was repeated 10 times in accordance with (-2 method), and the degree of fibril was observed with an electron microscope. Almost no fibrillation was observed in any of the samples.

[0028]

[Table 2]

Example 3 Tencel (a fineness of 1.5 d, length of 38 mm) manufactured by Coatles Co., Ltd., which is a solvent-spun cellulose fiber, was spun into a 40-th yarn to produce a knit of Amanasa.

The nit was immersed in an aqueous solution of an enzyme having the formulation shown in Table 3 below, and was heated to a cellulase activation temperature of 50 to 55.
Treated at 60 ° C for 60 minutes. The pH of the aqueous enzyme solution was adjusted to 5 to 5.5 with a buffer.

At this stage, JIS L 0217 (103
Was repeated 10 times, and the degree of fibrillation was observed with an electron microscope. The results show that, as shown in Table 3 below, fibrillation cannot be completely prevented only by enzyme processing.

[0032]

[Table 3]

Next, the enzyme-treated nit is immersed in an aqueous solution of an N-methylolated amine compound having the following formulation, squeezed to 100% pick-up with a mangle, dried, and baked at 160 ° C. for 90 seconds. Was.

[0034] The obtained treated cloth is subjected to 1 according to JIS L 0217 (103 method).
Washing was repeated 0 times, and the degree of fibrillation was observed by an electron microscope. As a result, almost no fibrillation was observed.

Claims (1)

(57) [Claims] A solvent-spun cellulosic fiber is N-
A method for preventing fibrillation of solvent-spun cellulosic fibers, characterized by treating with a methylolated amine compound.