JPS6015747B2 - Method for manufacturing fiber structures - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention is a method for producing a fibrous structure, and more specifically, a structure containing 2% or more by weight of composite fibers consisting of polyolefin and polyester is treated with a non-solvent system to produce polyolefin. The present invention relates to a method for manufacturing a fiber structure that can be easily removed.

Traditionally, structures were made from composite fibers consisting of two or more components.
The subsequent removal of one component is currently being carried out for the following purposes.

■ When obtaining ultrafine fibers, direct spinning and drawing often causes problems such as fuzz and yarn breakage, so after drawing grade yarns as sea-island structure fibers, the sea component is extracted and removed to obtain ultrafine fibers.

■ Sea component of sea-island structure fiber or conjugate fiber 1
Effectively utilize the presence of ingredients to simplify the process.

For example, sea ingredients can be used in place of sizing agents or adhesives and used as threads with special properties. ■ Manufacturing, spinning, weaving, and weaving of ultrafine fibers or special cross-section fiber sheets and nonwoven fabrics are difficult, so after manufacturing structures using sea-island structural fibers or conjugate fibers, one component, which is polyolefin, is separated and removed. A sheet, nonwoven fabric, woven fabric, or knitted fabric made of ultrafine fibers or fibers with a special cross section is obtained.

Conventionally, methods for removing these polyolefins have been extraction methods using organic solvents such as tetrachloroethylene, trichlorethylene, toluene, xylene, n-heptane, etc., taking advantage of the difference in solvent extractability from polyesters.
There are problems of toxicity and danger due to organic solvents, as well as problems of recovery and environmental pollution, and in order to conduct these on an industrial scale, equipment that solves the above problems and sufficient operational management are required.
In addition, as seen in Tokubatsu 13620-1980, a composite fabric consisting of two components or its structure is coated with a surfactant, and then treated with an aqueous solution of phenol, benzine alcohol, etc. to separate the two components and form fibrils. However, there is no method to completely separate and remove one component of polyolefin by dispersing it in an aqueous solution using only an aqueous surfactant solution as in the present invention. As a result of extensive research over many years, the present inventors have discovered an innovative method for removing one component using an aqueous system that is completely non-toxic and dangerous and does not require any special equipment.

That is, a structure containing 2% by weight or more of composite fibers in which one component A is polyolefin and the other component B is polyester is immersed in an aqueous solution containing 0.01% by weight or more of a surfactant, and then placed under the foot of Azusa. It has been surprisingly discovered that polyolefins can be removed from structures by treatment with an aqueous solution at a temperature higher than the melting point of component A and lower than the melting point of component B.

According to this method, toxicity and danger when using organic solvents,
There are no problems such as environmental pollution or corrosion of containers.
It is possible to manufacture fiber structures by removing polyolefins using ordinary high-pressure containers, such as high-temperature dyeing machines for polyester woven and knitted fabrics, high-temperature relaxers, etc., and the removed polyolefins float in the aqueous solution in the form of particles. Therefore, it is a completely new and revolutionary method that requires only a simple separation operation and does not require any recovery equipment, and unlike solvent extraction, it is possible to completely remove one component in a single batch method. It is. The polyester polymer referred to in the present invention refers to aromatic dicarboxylic acids such as terephthalic acid, isophthalic acid, and naphthalene-2,6-dicarboxylic acid, aliphatic dicarboxylic acids such as adipic acid and sebacic acid, or esters thereof, and ethylene glycol and diethylene glycol. , 1,4-butanediol, neobentyl glycol, dichlorohexane, 1,4-dimethanol, and other diol compounds, and refers to a polyester in which 75% or more of the repeating units are polyethylene terephthalate.

In particular, aliphatic or aromatic compounds, primary to quaternary amine compounds containing metal salts of sulfonic acid, carbonic acid, phosphoric acid, or carboxylic acid to facilitate separation of polyolefin and polyester in an aqueous surfactant solution. , acid amide compounds, polyalkylene oxide compounds, etc. are preferably copolymerized or/and blended (kneaded) with polyethylene terephthalate in an amount of 1 to 20 mol %, and more preferable compounds include dicarboxylic acids, alkyl groups, alkyl ethers, and alkyl ethers. There are metal salts of sulfonic acid, carbonic acid, phosphoric acid or carboxylic acid of ster, as well as polyalkylene oxides having a molecular weight of 500 to 50,000 and having groups or groups or alkylamine groups.

On the other hand, the polyolefin referred to in the present invention is polyethylene,
It means polypropylene, etc., and more preferably low density polyethylene with a low melting point.

The composite fibers referred to in the present invention are, for example, known side/side type, core-sheath type composite fibers, chip blend method,
Umejima structural fibers obtained by a multi-layered-jointed-divided melt-mixing method or a multi-core-to-sheath composite weaving method are included, and examples of the fiber cross sections are shown in FIGS. 1 to 8. In the figure, the shaded area indicates polyester, which is the non-removed component B. In the present invention, a structure containing 2% by weight or more of the above-mentioned composite weave is soaked in an aqueous surfactant solution of 0.01% by weight or more, and heated to a temperature equal to or higher than the melting point of the removed component A and the non-removed component B. or after treatment with an aqueous surfactant solution, the surfactant is finally reduced to 0.
．． In water to form an aqueous solution containing 0.1% by weight or more, the polyolefin of component A is treated under temperature at a temperature higher than the melting point of component A and lower than the melting point of component B. In either method, as a result, the polyolefin of component A becomes a component of B. is separated from the polyester and floats in the aqueous solution. In this case, if the treatment is carried out at a temperature below the melting point of the polyolefin, the polyolefin will remain fixed to the polyester and will not separate, thereby losing the effect of the present invention. In addition, from the viewpoint of damage to the polyester fibers, it is desirable that the temperature be higher than the melting point of polyolefin and as low as possible to remove the polyolefin. The concentration of the surfactant in the aqueous solution is preferably 0.01% by weight or more, more preferably 0.1 to 10% by weight. If it is less than 0.01% by weight, it will be difficult to remove the polyolefin, requiring long-term treatment at high temperatures, and it will not be possible to remove it with water alone.

Further, if the amount of surfactant is unnecessarily large, it is not preferable because it takes time to clean the structure after removing the polyolefin and the loss of surfactant becomes large. In addition, when the amount of composite fibers is less than 2% by weight, it is difficult to exhibit the characteristics of a fiber structure in which one component is removed. Anionic, cationic, nonionic, and amphoteric surfactants can be used as surfactants, but if the polyester modifier is anionic, anionic, nonionic, and amphoteric surfactants other than cationic surfactants can be used for polyolefin. It greatly contributes to the removal effect,
When the modifier is cationic, cationic, nonionic and amphoteric surfactants are preferred. Further, it is preferable that the surfactant adhering to the fibrous structure after polyolefin removal be easily removed by washing with water or washing with a moat. Examples of anionic surfactants include organic compounds containing fatty acid salts, sulfate ester salts, sulfonate salts, or phosphate ester salts.
Examples of cationic surfactants include organic compounds containing quaternary ammonium salts or higher amine salts, examples of ionic surfactants include organic compounds of polyethylene glycol type or polyhydric alcohol type, and amphoteric surfactants. For example, it means a carboxylate type, sulfate ester salt type, sulfonate type, or phosphate ester salt type of quaternary amine compound. Further, the surfactant is used after being dissolved or emulsified in water, but it is also possible to use it in a mixed system to maintain this state. Furthermore, in order to remove polyolefin, mechanical vibration, ultrasonic vibration, solution jetting, etc., in short, are necessary. This movement may be any state in which it moves relative to either the aqueous solution or the composite fiber, and more preferably means a state in which both move together. For example, a dyeing machine, a relaxer, a scouring machine, etc. are suitable as a means for treating the material in an aqueous solution with such fly lye. The bath ratio used is 1:15 or more, preferably 1:30 to 10 Tochihata. The fibrous structure referred to in the present invention refers to woven or knitted fabrics manufactured from fibrous materials. Nonwoven fabrics, paper, etc.
In this case, it also includes peaches containing 30% or less of materials other than fibers, such as resins and sizing agents, and refers to structures from which polyolefin has been substantially removed.

In the present invention, "substantially removed" means that the amount of residual polyolefin is reduced to 3% or less of the structure. The above-mentioned fibrous structure is used, for example, as a product with a normal beam color finish, a raised product with a raised and finished finish, or an artificial leather coated with a resin or the like.

Hereinafter, the method of the present invention will be specifically explained with reference to Examples.

Example 1 As an island component, [ri] = 0.60 so/min (intrinsic viscosity measured using an Ubbelohde viscometer in a constant temperature bath at 30 qo using a mixed solvent of equal amounts of phenol and tetrachloroethane)
Polyethylene terephthalate is used as the sea component, and polyethylene with a melting point of 115 qo produced by a high-pressure method is used as a sea-island component ratio of 2:3, and a sea-island structure fiber with an island average denier of 0.1 is manufactured by a special mixed grade yarn method to produce 500 denier. 150 denier polyester processed thread is used for the warp thread, the density of the thread is 6 t/inch, and the density of the warp thread is 91.
This is made up of 3 pieces of 5 pieces of chocolate satin fabric.

In this case, the sea-island structure fibers account for 65% of the total weight of the fabric, and this fabric was treated with a 5% aqueous solution of POE {71 lauryl ether (7 moles of ethylene oxide adduct of lauryl alcohol) at 125°C for 2 hours using a solution injection type device. Then, the polyethylene separated from the polyester and floated in the form of particles in the aqueous solution. Next, the woven fabric was washed with water to remove the nonionic surfactant, dried, and then raised using a needle cloth raising machine and given a beam color finish to obtain a natural-like suede fabric. In addition, the polyethylene was completely extracted from the fabric after surfactant treatment, water washing, and drying using 7.0% perchloren, and the residual percentage of polyethylene was calculated from the change in weight of the fabric before and after extraction. .2% by weight. Example 2 [
= 0.6 Sodium sulfonate of dimethyl isophthalic acid is added to polyethylene terephthalate.
．． 5 mol% copolymerized material was used as the island component, and the sea component was high-density polyethylene with a melting point of 130°C.The sea-island component ratio was 1.
Sea-island structure fiber with island average denier of 0.7 in pair 2 is processed using special mixed grade yarn method. It is made from 250 denier and used as the front yarn of the tricot knit, and the back yarn is 10 denier.
A striped fabric with long floats was constructed using 0 denier processed polyester yarn.

Sea-island structure fibers account for 50% of the total weight of the knitted fabric*
was treated with the following surfactant aqueous solution at 150° C. for 1 hour in a high-pressure container with a kneading effect, then washed in a moat and dried. The polyethylene removal results are shown in Table 1. Table 1 *Polyethylene residual rate indicates the percentage of the total knitted fabric weight K after surfactant treatment, hot water washing, and drying.

Example 3 〔〔〔〕=0.62゜/The polyethylene terephthalate (molecular weight 20,000) was added at 1% by weight.
3:2 ratio of kneaded material and polyethylene with melting point of 120℃
Composite fibers were made in a side-by-side type, and a 50-denier plain-woven fabric was constructed.

The obtained fabric was treated with the following surfactant aqueous solution under various conditions in a solution reflux type high-pressure container, washed in a moat, and dried to obtain a polyester lining with an irregular cross section. The results are shown in Table 2. Table 2 Example 4 Adduct of polypropylene glycol poly'ethylene oxide of laurylamine to Kunota's polyethylene terephthalate with [ri] = 0.7 (q2 days, 2 days, 2 days) % copolymerized as an island component, and polyethylene with a melting point of 110° C. as a sea component, a sea-island structure fiber was produced by a chip blending method.

Next, a random web was prepared from the fibers and polyurethane was impregnated therein, and then treated with a 1% aqueous solution of lauryltrimethylammonium chloride in a pressure vessel while applying ultrasonic vibration for 2 hours at 120 qo. was completely separated from the polyester and floated in the form of particles in the aqueous solution. Next, the nonwoven fabric was washed with water, dried, and then the surface was fluffed with sandpaper and dyed to obtain a suede finish. Example 5 Pentaerythritol 0.25 mol% and methoxypolyethylene gelicol (CH30-(CQC day 2
0) n day and n = 30 to 45) was copolymerized with 0.5 mol% as the island component, and polypropylene with a melting point of 160°C was used as the sea component to produce an island average denier of 0 using a special moat joint spinning method.
．． A sea-island structure fiber of No. 3 was manufactured.

Next, the fibers were made into 1,000 denier and tufted onto a polyester base fabric having a basis weight of 350 denier under the conditions of a gauge of 1'8 inches, a stitch rate of 1q folds/inch, and a pile length of 5 skins to form a pile fabric band. The fabric was previously treated with a 20% aqueous solution of POE15 stearate, and
After drying for 1 minute to deposit 1% by weight of the surfactant, it was treated with a 170°C aqueous solution for 2 hours in a solution injection type high-pressure vessel, and the polypropylene separated from the polyester and became granular in the aqueous solution. It surfaced. Next, the cloth was washed with hot water to remove the anionic surfactant and dried to obtain a pile cloth. The polypropylene residual rate was 1.2% by weight. Brief explanation of the drawings Figures 1 to 8, which are shown as drawings, are all cross-sectional views of various composite fibers that can be used in the present invention. The other part is a polyolefin component.

Figure 1 Traditional 2 illustrations Figure 3 Figure 4 Figure 5 Figure 6 Figure 7 Figure 8

Claims (1)

[Scope of Claims] 1 A fiber structure containing 20% by weight or more of a conjugate fiber in which one component A is polyolefin and the other component B is polyester, and the final surfactant is 0.01% by weight or more. immersed in water at a temperature higher than the melting point of component A under stirring,
A method for producing a fibrous structure, characterized in that component A is removed by treatment at a temperature below the melting point of component B. 2. The method for producing a fibrous structure according to claim 1, characterized in that the fibrous structure is immersed in an aqueous solution containing 0.01% by weight or more of an active surfactant and treated under stirring. 3. The fibrous structure is treated in advance with an aqueous surfactant solution, and then treated under stirring in water to finally form an aqueous solution containing 0.01% by weight or more of the surfactant. A method for producing a fibrous structure according to item 1.