JP6339861B2 - Filling, and futon and garment containing the filling - Google Patents

Description

  The present invention relates to a batting containing feathers and cross-linked acrylate fibers, and a futon and a garment containing the batting.

  Feathers have high heat retention properties and are widely used as batting for bedding and clothing. However, prices have soared with increasing demand in recent years and the epidemic of avian influenza. On the other hand, if fibers other than feathers can be used in combination, costs can be reduced. However, when the amount of feathers decreases, the heat retention decreases. As a method for compensating for this, it is conceivable to use in combination with a fiber having hygroscopic heat generation.

  For example, Patent Document 1 discloses a moisture absorbing / releasing exothermic heat-retaining product using a batting in which animal fibers such as feathers and a cross-linked acrylate fiber that is a moisture absorbing / releasing exothermic fiber are mixed. Such padding can be heated and kept warm by absorbing moisture in the gas phase and liquid phase generated from the human body. However, since the cross-linked acrylate fiber is likely to be entangled between fibers in the production process and difficult to open, it is difficult to uniformly mix the feathers and the cross-linked acrylate fiber, and the appearance of the batting can be spotted, It tends to be inferior in quality. Further, when washing or the like is performed, the entanglement is further increased, and a foreign object sensation and thickness spots are generated. In addition, non-uniform mixing tends to lower the functions such as heat retention due to moisture absorption heat generation.

  Patent Document 2 discloses a method for producing short cotton mixed feather cotton. In such a method, it is possible to uniformly mix short fibers and feathers. However, as described above, the crosslinked acrylate fiber has a property that it is difficult to open, so even if these methods are used, it is not easy to uniformly mix the crosslinked acrylate fiber with feathers.

Japanese Patent Laid-Open No. 11-12833 JP-A-10-219526

  As described above, it is not easy to uniformly mix feathers and cross-linked acrylate fibers. The present invention has been made in view of the current state of the prior art, and has a feeling of foreign matter, a small thickness unevenness, a cotton pad in which feathers and crosslinked acrylate fibers are uniformly mixed, and bedding and clothing using the cotton pad. The purpose is to provide.

That is, the above object of the present invention is achieved by the following means.
(1) A filling containing feathers and cross-linked acrylate fibers, wherein the ratio of twisted cotton contained in the filling is 5% by weight or less, and the number of twisted cotton contained in 1 g of filling is 8 or less. And a ratio of crimp ratio / crimp number of the crosslinked acrylate fiber is 0.60% · inch / piece or less .
( 2 ) The filling according to ( 1), wherein the crosslinked acrylate fiber contains 4.5 to 8 mmol / g of a salt-type carboxyl group.
( 3 ) The crosslinked acrylate fiber is obtained by subjecting a towed acrylonitrile fiber to a crosslinking treatment and a hydrolysis treatment with a nitrogen-containing compound having two or more nitrogen atoms in one molecule. The filling according to (1) or (2 ), wherein
( 4 ) A bedding comprising the batting according to any one of (1) to ( 3 ).
( 5 ) A garment comprising the batting according to any one of (1) to ( 3 ).

  The batting of the present invention has a small content of twisted cotton, and feathers and cross-linked acrylate fibers are uniformly mixed. The feather / cross-linked acrylate fiber mixed batting of the present invention can be used as a substitute for feather batting because there is little foreign matter feeling and thickness unevenness, and the heat-absorbing heat generation performance of the cross-linked acrylate fiber can also compensate. is there. Specifically, it can be suitably used as a futon or batting for clothing.

  The batting of the present invention is a batting containing feathers and cross-linked acrylate fibers, and the proportion of twisted cotton contained in the batting is 5% by weight or less, more preferably 4% by weight or less, still more preferably 3% by weight. It is as follows. Further, the number of twisted cotton contained per 1 g of batting is 8 or less, more preferably 5 or less, and still more preferably 3 or less. Here, the twisted cotton is a portion in which the fibers are entangled with each other in the batting. If the ratio of the twisted cotton in the filling measured by the method described later is 5% by weight or less and the number of the twisted cotton is 8 or less, the padding practically feels no foreign matter or thick spots. It becomes. Such twisted cotton is considered to be mainly caused by poor opening of the crosslinked acrylate fiber.

  There is no restriction | limiting in particular as a feather employ | adopted for the batting of this invention, The mixing rate of a down and a feather is not prescribed | regulated. Further, it may be goose, duck, or other. Further, the batting of the present invention may contain a maximum of 50% by weight of fibers other than feathers and cross-linked acrylate fibers described later. As such fiber, natural fiber, regenerated fiber, semi-synthetic fiber, synthetic fiber, etc. can be used. As natural fiber, cotton, silk, wool, as regenerated fiber, rayon, cupra, tencel, lyocell, semi-synthetic. Examples of the fiber include acetate, triacetate, promix, and examples of the synthetic fiber include polyester, nylon, polyethylene, polypropylene, polyurethane, polyvinyl alcohol, and acrylic.

  The cross-linked acrylate fiber employed in the batting of the present invention is a fiber composed of a polymer containing a carboxyl group and a cross-linked structure. Such a polymer having a carboxyl group and a crosslinked structure is obtained by subjecting a fiber made of an acrylonitrile polymer to a crosslinking treatment with a nitrogen-containing compound having two or more nitrogen atoms in one molecule, and a hydrolysis treatment. Things can be mentioned.

  Here, the nitrogen-containing compound having two or more nitrogen atoms in one molecule is preferably an amino compound or a hydrazine-based compound having two or more primary amino groups. The upper limit of the number of nitrogen atoms in one molecule is not particularly limited, but is preferably 12 or less, more preferably 6 or less, and particularly preferably 4 or less. When the number of nitrogen atoms in one molecule exceeds the above upper limit, the cross-linking agent molecule becomes large and it may be difficult to introduce cross-linking into the polymer.

  Examples of amino compounds having two or more primary amino groups include diamine compounds such as ethylenediamine and hexamethylenediamine, diethylenetriamine, 3,3′-iminobis (propylamine), N-methyl-3,3′-iminobis ( Triamine compounds such as propylamine), triethylenetetramine, N, N′-bis (3-aminopropyl) -1,3-propylenediamine, N, N′-bis (3-aminopropyl) -1,4- Examples include tetramine compounds such as butylenediamine, polyamine compounds having two or more primary amino groups such as polyvinylamine and polyallylamine.

  Examples of the hydrazine compound include hydrazine hydrate, hydrazine sulfate, hydrazine hydrochloride, hydrazine hydrobromide, hydrazine carbonate, and the like.

  Further, the carboxyl group amount is preferably 0.1 to 10 mmol / g, more preferably 0.5 to 8 mmol / g, still more preferably 3 to 8 mmol / g based on the fiber weight. When the amount of carboxyl groups is less than 0.1 mmol / g, functions such as moisture absorption exothermic properties and deodorizing properties described later may not be sufficiently obtained. In addition, when the carboxyl group amount exceeds 10 mmol / g, the cross-linked structure is inevitably reduced, and the fiber becomes brittle due to swelling due to water absorption, making it difficult to maintain practical fiber strength and elongation. is there.

  As the state of the carboxyl group, if the counter ion is H, that is, in the form of COOH (hereinafter also referred to as H-type carboxyl group), in particular, deodorizing performance such as ammonia gas such as ammonia, triethylamine, pyridine, etc. and antiviral Excellent performance in terms of performance, anti-allergen performance and antibacterial performance. Regarding the anti-allergen performance, the allergen to be removed is not particularly limited, but allergens generated from pollen, mites and the like can be efficiently removed.

  If the type of the counter ion of the carboxyl group is a cation other than H (hereinafter also referred to as a salt-type carboxyl group), excellent deodorizing performance and absorption / release for acid gases such as acetic acid and isovaleric acid, and aldehydes such as formaldehyde Wet performance is expressed. Moreover, a high effect can be acquired also regarding a flame retardance performance, antiviral performance, antiallergen performance, and antimicrobial performance. Examples of the cation constituting such a salt-type carboxyl group include alkali metals such as Li, Na and K, alkaline earth metals such as Be, Ca and Ba, Cu, Zn, Al, Mn, Ag, Fe and Co. , A metal such as Ni, a cation such as NH 4, or an amine, and a plurality of types of cations may be mixed.

  Here, when emphasizing the hygroscopic heat generation performance, the salt-type carboxyl group amount is preferably 4.5 mmol / g or more. As the kind of cation, Na, K, Mg, Ca, Al, Zn or the like can be preferably used. Further, the upper limit of the salt-type carboxyl group amount is desirably 8 mmol / g or less from the viewpoint of maintaining practical fiber strength and elongation.

The cross-linked acrylate fiber employed in the present invention has a crimp ratio / crimp number ratio of 0.60 % · inch / piece or less, preferably 0.50 % · inch / piece or less, more preferably 0.30 %. -Those having an inch / piece or less. The ratio of crimp ratio / crimp number is an index of the size of each wave shape caused by crimp. The smaller this value, the smaller the size of each wave shape due to crimping. The cross-linked acrylate fiber employed in the present invention has a value of such an index of 0.60 % · inch / piece or less, and since the wave shape is small, the single fibers of the cross-linked acrylate fiber are not easily entangled with each other. The characteristic is obtained. Due to this feature, the cross-linked acrylate fiber employed in the present invention can be easily dispersed in a single fiber and can be easily and uniformly mixed with other fibers such as feathers. On the other hand, the lower limit of the ratio of crimp ratio / crimp number is preferably 0.10 % · inch / piece or more. When such a ratio is less than 0.1 % · inch / piece , it can be easily and uniformly mixed with other fibers such as feathers, but the entanglement with other fibers becomes too small, and cross-linking occurs due to use or washing. Acrylate fibers are easily removed from other fibers.

  The crimp rate of the crosslinked acrylate fiber employed in the present invention is preferably 4% or less. If the crimp rate is too large, it may be difficult to open the single fibers. The lower limit of the crimp rate is preferably 1% or more. If the crimping ratio is too small, the entanglement with other fibers becomes too small, and the crosslinked acrylate fiber may easily fall off from other fibers due to use or washing.

  Further, in terms of facilitating dispersion in a single fiber and allowing easy uniform mixing with other fibers, the fiber length of the crosslinked acrylate fiber employed in the present invention is preferably 13 mm or less, more preferably 8 mm or less. Is desirable. The lower limit of the fiber length is desirably 1 mm or more because if it is too short, it will fall off immediately even if mixed with other fibers and the mixed state cannot be maintained.

  As the moisture absorption performance of the crosslinked acrylate fiber of the present invention, when mixed with other fibers such as feathers, the moisture absorption rate described below is preferable from the viewpoint of obtaining significant moisture absorption performance or moisture absorption heat generation performance at a practical mixing ratio level. Is preferably 20% or more, more preferably 25% or more, and still more preferably 35% or more. The upper limit of the moisture absorption rate is not particularly limited. However, since there is a limit to the amount of carboxyl groups introduced, the upper limit is approximately 70%.

  Examples of the method for producing the crosslinked acrylate fiber of the present invention described above include a method of subjecting acrylonitrile fiber to a crosslinking treatment and a hydrolysis treatment with a nitrogen-containing compound having two or more nitrogen atoms in one molecule. be able to.

  In such a method, the acrylonitrile fiber is a fiber formed of an acrylonitrile polymer containing acrylonitrile in an amount of 40% by weight or more, preferably 50% by weight or more, and more preferably 80% by weight or more. Therefore, as the acrylonitrile-based polymer, a copolymer of acrylonitrile and another monomer can be employed in addition to the acrylonitrile homopolymer. Other monomers in the copolymer are not particularly limited, but vinyl halides and vinylidene halides; (meth) acrylic acid esters (note that (meth) is indicated with or without the word “meta”. Sulfonic acid group-containing monomers such as methallyl sulfonic acid and p-styrene sulfonic acid and salts thereof; carboxylic acid group-containing monomers such as (meth) acrylic acid and itaconic acid and salts thereof; acrylamide, styrene, Examples include vinyl acetate.

  An acrylonitrile fiber can be obtained by dissolving the acrylonitrile polymer in a solvent to obtain a spinning dope, and spinning the solution. There is no limitation on the spinning method and conditions, and spinning by a regular method can be used. Here, examples of the solvent for dissolving the acrylonitrile-based polymer include organic solvents such as dimethylformamide, dimethylacetamide, and dimethylsulfoxide, and inorganic salt solvents such as nitric acid, zinc chloride aqueous solution, and sodium thiocyanate aqueous solution.

  Next, the acrylonitrile fiber obtained as described above is subjected to the above-described crosslinking treatment with a nitrogen-containing compound having 2 or more nitrogen atoms in one molecule. The conditions for such crosslinking treatment are not limited as long as a crosslinked structure is formed, and preferable results can be obtained when acrylonitrile fibers are immersed in a solution of the nitrogen-containing compound and reacted at 50 to 150 ° C. However, when a hydrazine compound is used, the following conditions can be employed.

  That is, specific treatment conditions for the crosslinking treatment with the hydrazine compound can be adopted as long as the increase in the nitrogen content can be adjusted to 0.1 to 10% by weight, but the hydrazine compound concentration is 5 to 20% by weight. A means for treating in a 50% aqueous solution at a temperature of 50 to 110 ° C. for 1 to 5 hours is industrially preferred. Here, the increase in the nitrogen content refers to the difference between the nitrogen content of the acrylonitrile fiber before the crosslinking treatment with the hydrazine compound and the nitrogen content of the fiber after the treatment. If the increase in nitrogen content is less than the lower limit, fibers having physical properties that can be finally satisfied in practice may not be obtained. If the upper limit is exceeded, sufficient moisture absorption exothermicity or deodorization may not be obtained. Functions such as sex may not be obtained.

  The fiber subjected to the crosslinking treatment may be subjected to an acid treatment after sufficiently removing the drug remaining by the treatment. Examples of the acid used here include mineral acids such as nitric acid, sulfuric acid, and hydrochloric acid, and organic acids, but are not particularly limited. The conditions for the acid treatment are not particularly limited, but the fibers are usually immersed in an aqueous solution having an acid concentration of 3 to 20% by weight, preferably 7 to 15% by weight, at a temperature of 50 to 120 ° C. for 0.5 to 10 hours. An example is given.

  The fiber subjected to the crosslinking treatment as described above or the fiber further subjected to the acid treatment is then subjected to a hydrolysis treatment. By this treatment, nitrile groups remaining unreacted during the crosslinking treatment are hydrolyzed to generate carboxyl groups.

  As a means for such hydrolysis treatment, a basic aqueous solution such as alkali metal hydroxide, alkali metal carbonate, ammonia, or a state in which a fiber subjected to crosslinking treatment is immersed in an aqueous solution such as nitric acid, sulfuric acid, hydrochloric acid, etc. And a means for heat treatment. Specific processing conditions may be set as appropriate in consideration of the amount of the target carboxyl group and the like, and various conditions such as the concentration of the processing agent, reaction temperature, reaction time, etc., but preferably 0.5 to 10 weights. %, More preferably, means for treating at a temperature of 50 to 120 ° C. for 1 to 10 hours in an aqueous treatment chemical solution of 0.5 to 2.5% by weight is also preferred in terms of industrial and fiber properties. In addition, a hydrolysis process can also be performed simultaneously with the crosslinking process mentioned above.

  The fiber hydrolyzed as described above may then be acid treated. When a basic aqueous solution such as an alkali metal hydroxide, alkali metal carbonate, or ammonia is used in the hydrolysis treatment, the generated carboxyl group forms an ionic bond with a cation such as an alkali metal. By the acid treatment, such a cation is replaced with a hydrogen ion to form an H-type carboxyl group. As a means for such acid treatment, a method of immersing the hydrolyzed fiber in an acidic aqueous solution such as hydrochloric acid, acetic acid, nitric acid, sulfuric acid, etc., and then drying is suitably used.

  Furthermore, if the fiber subjected to acid treatment as described above is subjected to ion exchange treatment with an aqueous metal salt solution such as nitrate, sulfate, or hydrochloride according to the required characteristics, the desired metal ion is counter-ionized. It can be made into the salt type carboxyl group. Furthermore, by adjusting the pH of the aqueous solution and the concentration and type of the metal salt, it is possible to mix different types of counter ions and to adjust the ratio thereof.

In the production method described above, from the viewpoint of setting the ratio of the crimp ratio / crimp number of the finally obtained crosslinked acrylate fiber to the above-mentioned range, the crimp ratio / crimp of the acrylonitrile fiber used as the raw material of the fiber The reduction ratio is preferably 0.80 % · inch / piece or less, more preferably 0.75 % · inch / piece or less. The lower limit of the ratio is preferably 0.10 % · inch / piece or more. As a method of setting such a ratio of crimp ratio / crimp number, there are methods of adjusting the conditions of the crimp application process in the general production process of acrylonitrile fiber, or omitting the crimp application process after the heat treatment. Can be mentioned.

  Further, it is desirable that the acrylonitrile fiber is subjected to the above-described crosslinking treatment and hydrolysis treatment in a tow state, that is, in a state where the acrylonitrile fiber is not cut into short fibers. When each treatment is performed in the tow state, the fibers are restrained to some extent even in the treatment bath, so that entanglement due to the liquid flow is less likely to occur, and in the subsequent fiber removal process, etc. It is considered that crimping is stretched and the crimping rate tends to be smaller because tension is applied.

  Further, when the acrylonitrile fiber in the tow state is subjected to a treatment such as a crosslinking treatment or a hydrolysis treatment, it is cut into short fibers after these treatments. In this case, there is also an advantage that the variation in the fiber length of the short fiber is reduced as compared with the case where these treatments are performed after the acrylonitrile fiber is cut into short fibers.

  As a use ratio of the feather and the cross-linked acrylate fiber in the batting of the present invention, it is desirable that the feather is 50 to 95% by weight and the cross-linked acrylate fiber is 5 to 50% by weight based on the weight of the batting. Further, as described above, fibers other than feathers and cross-linked acrylate fibers can be mixed up to a maximum of 50% by weight of the batting.

  As a method for producing the batting of the present invention, while stirring an aqueous dispersion composed of feathers and water, an aqueous dispersion composed of a cross-linked acrylate fiber is added thereto, and the mixture is stirred so as to be uniformly dispersed, followed by dehydration and drying. The method by performing can be mentioned. Here, as the cross-linked acrylate fiber, one that is not in a water-dispersed state but in a wet state that is not subjected to a fiber opening treatment may be added.

  The above-described batting of the present invention has less foreign material feeling and thickness unevenness, and can retain heat retention due to the hygroscopic heat generation performance of the crosslinked acrylate fiber, so that it can be used for the same use as a feather batting and is expensive. The amount of feathers used can be reduced. Also, since there is no difference in handling from a feather pad, it can be processed by the same method as a feather pad. Examples of suitable uses of the batting of the present invention include bedding and clothing. Examples of the bedding include a futon, a pillow, a sleeping bag, and a kotatsu futon. Examples of the clothing include a winter clothes, a down jacket, and ski wear.

  Hereinafter, the present invention will be described specifically by way of examples. Parts and percentages in the examples are on a weight basis unless otherwise indicated. The evaluation method of characteristics in the examples is as follows.

(1) Ratio of crimp ratio / crimp number Measured according to JIS-L1015. The ratio of crimp ratio / crimp number is calculated from the obtained crimp ratio [%] and the number of crimps [pieces / inch].

(2) Amount of carboxyl group About 1 g of a fiber sample is immersed in 50 ml of a 1 mol / l hydrochloric acid aqueous solution for 30 minutes. The fiber sample is then immersed in water at a bath ratio of 1: 500. When it is confirmed that the bath pH is 4 or more after 15 minutes, the bath is dried (if the bath pH is less than 4, it is washed again with water). Next, about 0.2 g of a sufficiently dried fiber sample is precisely weighed (W1 [g]), 100 ml of water is added, and 15 ml of a 0.1 mol / l sodium hydroxide aqueous solution and 0.4 g of sodium chloride are added. And add phenolphthalein and stir. After 15 minutes, the sample fibers and filtrate are separated by filtration, and the sample fibers are subsequently washed with water until there is no coloration of phenolphthalein. The combined washing water and filtrate at this time are titrated with 0.1 mol / l hydrochloric acid aqueous solution until the phenolphthalein is no longer colored, and the aqueous hydrochloric acid consumption (V1 [ml]) is determined. From the obtained measured value, the total carboxyl group amount is calculated by the following formula.
Amount of carboxyl group [mmol / g] = (0.1 × 15−0.1 × V1) / W1

  In the above method for measuring the amount of carboxyl groups, the amount of H-type carboxyl groups is calculated in the same manner except that the first immersion in 1 mol / l hydrochloric acid aqueous solution and subsequent water washing are not performed. The amount of salt-type carboxyl groups is calculated by subtracting the amount of H-type carboxyl groups from the total amount of carboxyl groups.

(3) 20 ° C. × 65% RH moisture absorption About 2.5 g of the fiber sample is dried with a hot air dryer at 105 ° C. for 16 hours, and the weight is measured (W2 [g]). Next, the fiber sample is placed in a thermo-hygrostat adjusted to a temperature of 20 ° C. and 65% RH for 24 hours. The weight of the fiber sample thus absorbed is measured (W3 [g]). From these measurement results, a 20 ° C. × 65% RH moisture absorption rate is calculated by the following equation.
20 ° C. × 65% RH moisture absorption [%] = (W3−W2) / W2 × 100

(4) Dispersibility About 5 g of a measurement sample is collected from the sample batting and the weight (W4 [g]) is measured. The collected batting is visually observed, and a portion where the fiber sample is entangled and formed into a lump, that is, a poorly dispersed portion is separated. Further, the number (N1 [pieces]) and weight (W5 [g]) of the separated fiber samples are measured, and the number and weight ratio per 1 g of the poorly dispersed portion are calculated by the following formula.
Number of defective dispersion portions per 1 g [piece / g] = N1 / W4
Weight ratio [%] of poorly dispersed portion = W5 / W4 × 100
The above procedure is repeated three times, the average value of the number of unnecessary portions and the weight is obtained, and the dispersibility of the filling is evaluated.
Moreover, the foreign material feeling when touching the hand was evaluated according to the following criteria.
○: There is no sense of foreign matter △: There is almost no sense of foreign matter ×: There is a clear sense of foreign matter

[Production Example 1]
Acrylonitrile polymer Ap (90% by weight of acrylonitrile and 10% by weight of acrylic acid methyl ester) (Intrinsic viscosity [η] = 1.5 in dimethylformamide at 30 ° C.) was dissolved in 48% aqueous Rhodan soda solution to prepare a spinning dope. Prepared. Using the spinning dope, spinning was performed according to a conventional method, and an acrylonitrile fiber having a single fiber fineness of 0.9 dtex was obtained in a tow state without being cut. The ratio of the crimp ratio / crimp number of the acrylonitrile fiber was adjusted to 0.71 % · inch / piece by adjusting the conditions of the crimping step in spinning.

  The towed acrylonitrile fiber was subjected to a crosslinking introduction treatment at 98 ° C. for 5 hours in a 20% aqueous solution of hydrazine hydrate and washed. The cross-linked fiber was immersed in a 3% nitric acid aqueous solution and subjected to acid treatment at 90 ° C. for 2 hours. Then, it hydrolyzed at 90 degreeC x 2 hours in 3% sodium hydroxide aqueous solution, processed with 3.5% nitric acid aqueous solution, washed with water, and dehydrated. Subsequently, the fiber of the manufacture example 1 which has Na salt type carboxyl group was obtained by pulling out the fiber of a tow | toe state, cut | disconnecting in a short fiber shape, and drying. The evaluation results of the obtained fiber are shown in Table 1.

[Production Example 2]
The towed acrylonitrile fiber obtained in Production Example 1 was subjected to crosslinking introduction treatment at 98 ° C. for 5 hours in a 20% aqueous solution of hydrazine hydrate and washed. The cross-linked fiber was immersed in a 3% nitric acid aqueous solution and subjected to acid treatment at 90 ° C. for 2 hours. Then, it hydrolyzed at 90 degreeC x 2 hours in 3% sodium hydroxide aqueous solution, processed with 3.5% nitric acid aqueous solution, and washed with water. The obtained fiber is immersed in water, adjusted to pH 11 by adding sodium hydroxide, and then immersed in an aqueous solution in which magnesium nitrate corresponding to twice the amount of carboxyl groups contained in the fiber is dissolved at 50 ° C. for 1 hour. As a result, an ion exchange treatment was performed and dehydration was performed. Subsequently, the fiber of the manufacture example 2 which has Mg salt type carboxyl group was obtained by cut | disconnecting in a short fiber shape and drying. The evaluation results of the obtained fiber are shown in Table 1.

[Production Example 3]
Acrylonitrile polymer Ap (90% by weight of acrylonitrile and 10% by weight of acrylic acid methyl ester) (Intrinsic viscosity [η] = 1.5 in dimethylformamide at 30 ° C.) was dissolved in 48% aqueous Rhodan soda solution to prepare a spinning dope. Prepared. Using the spinning dope, spinning was performed according to a conventional method, and an acrylonitrile fiber having a single fiber fineness of 0.9 dtex was obtained in a tow state without being cut. The ratio of the crimp ratio / crimp number of the acrylonitrile fiber was adjusted to 0.62 % · inch / piece by adjusting the conditions of the crimping step in spinning.

  The towed acrylonitrile fiber was subjected to a crosslinking introduction treatment at 98 ° C. for 5 hours in a 20% aqueous solution of hydrazine hydrate and washed. The cross-linked fiber was immersed in a 3% nitric acid aqueous solution and subjected to acid treatment at 90 ° C. for 2 hours. Then, it hydrolyzed at 90 degreeC x 2 hours in 3% sodium hydroxide aqueous solution, processed with 3.5% nitric acid aqueous solution, washed with water, and dehydrated. Subsequently, the tow-like fiber was pulled out, cut into a short fiber shape, and dried to obtain a fiber of Production Example 3 having a Na salt-type carboxyl group. The evaluation results of the obtained fiber are shown in Table 1.

[Production Example 4]
Acrylonitrile polymer Ap (90% by weight of acrylonitrile and 10% by weight of acrylic acid methyl ester) (Intrinsic viscosity [η] = 1.5 in dimethylformamide at 30 ° C.) was dissolved in 48% aqueous Rhodan soda solution to prepare a spinning dope. Prepared. Using the spinning dope, spinning is carried out in accordance with a conventional method, cut into short fibers, and a single fiber fineness of 0.9 dtex and a crimp ratio / crimp number ratio of 0.91 % .inch / piece acrylonitrile fiber Got.

  The short-fiber acrylonitrile fiber was subjected to a crosslinking introduction treatment at 98 ° C. for 5 hours in a 20% aqueous solution of hydrazine hydrate and washed. The cross-linked fiber was immersed in a 3% nitric acid aqueous solution and subjected to acid treatment at 90 ° C. for 2 hours. Subsequently, a hydrolyzing treatment at 90 ° C. for 2 hours in a 3% sodium hydroxide aqueous solution, a treatment with a 3.5% nitric acid aqueous solution, washing with water, dehydration and drying to produce a production example having a Na salt type carboxyl group 4 fibers were obtained. The evaluation results of the obtained fiber are shown in Table 1.

[Production Example 5]
The fiber of Comparative Example 1 was immersed in water, adjusted to pH 11 by adding sodium hydroxide, and then dissolved in an aqueous solution in which magnesium nitrate corresponding to twice the amount of carboxyl groups contained in the fiber was dissolved at 50 ° C. for 1 hour. Ion exchange treatment was performed by soaking, dehydrating, and drying to obtain a fiber of Production Example 5 having an Mg salt-type carboxyl group. The evaluation results of the obtained fiber are shown in Table 1.

[Examples 1 to 3, Comparative Examples 1 and 2]
Prepare an aqueous dispersion consisting of 4 parts of washed feathers (85% white duck down, 15% feather) and 400 parts water. While stirring the aqueous dispersion, an aqueous dispersion composed of 1 part of the fibers of each production example cut to a fiber length of 6 mm and 100 parts of water is added thereto. After the addition, the mixture is stirred for 10 minutes, and then dehydrated and dried to obtain a cotton pad made of feathers and fibers of each production example. The evaluation results of the obtained batting are shown in Table 2.

As can be seen from Tables 1 and 2, in Examples 1 to 3, in which the ratio of crimp ratio / crimp number was 0.60 % · inch / piece or less, the ratio of twisted cotton was 5 A filling having no foreign matter feeling was obtained with the weight% or less and the number being 8 or less. On the other hand, in Comparative Examples 1 and 2 using a crosslinked acrylate fiber having a ratio of crimp number / crimp rate exceeding 0.60 % · inch / piece , the number and amount of poorly dispersed portions are large, and foreign matter is contained in the batting. There was a feeling.

  The feather / cross-linked acrylate fiber mixed batting of the present invention can be used as a substitute for feather batting because there is little foreign matter feeling and thickness unevenness, and heat retention can be compensated by the hygroscopic heat generation performance of the cross-linked acrylate fiber. It can be preferably used as a batting for a futon or clothing.

Claims (5)

A filling containing feathers and cross-linked acrylate fibers, wherein the ratio of twisted cotton contained in the filling is 5% by weight or less, and the number of twisted cotton contained in 1 g of filling is 8 or less , And a ratio of crimp ratio / crimp number of the crosslinked acrylate fiber is 0.60% · inch / piece or less . The batting according to claim 1, wherein the cross-linked acrylate fiber contains a salt-type carboxyl group of 4.5 to 8 mmol / g. The crosslinked acrylate fiber is obtained by subjecting a towed acrylonitrile fiber to a crosslinking treatment and a hydrolysis treatment with a nitrogen-containing compound having two or more nitrogen atoms in one molecule. The batting according to claim 1 or 2 , characterized in. A bedding comprising the batting according to any one of claims 1 to 3 . Clothing which contains the batting in any one of Claims 1-3 .