JP2003027318A - Weaving composed of regenerated collagen fiber - Google Patents

Abstract

PROBLEM TO BE SOLVED: To obtain a weaving which can be styled by a high-temperature hair iron and has high heat resistance by using a regenerated collagen fiber as a hair raw material replacing human hair. SOLUTION: This weaving is obtained from a regenerated collagen fiber and comprises the regenerated collagen fiber having <=5% shrinkage percentage during the use of a hair iron at 160 deg.C. Further, preferably the regenerated collagen fiber is obtained by a wet-heat treatment at 40-140 deg.C. Further, preferably the regenerated collagen fiber is treated with a monofunctional epoxy compound and an aluminum salt.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to weaving made of regenerated collagen fibers, and more particularly to weaving having high heat resistance, which enables styling with a high temperature hair iron.

[0002]

2. Description of the Related Art In the field of weaving products, human hair is optimally and widely used as a raw material for hair due to the nature of the product. However, as a result of changes in women's hairstyles in recent years, due to the overall shortening of hair and the increase in permanent wave-treated hair,
It is difficult to secure the quantity of straight and long human hair suitable for human hair raw material. In particular, it is almost impossible to obtain raw materials of good quality and uniform length. Therefore, it has been attempted to use synthetic fibers such as modacrylic fiber, vinyl chloride fiber, polyester fiber, and polypropylene fiber as a raw material for replacing human hair. The styling causes shrinkage, melting, or deformation of the hair tips, and has not yet fully achieved the purpose of replacing human hair. In addition, human hair currently in use has undergone many treatment processes such as sterilization, decolorization, dyeing, and gloss imparting, starting with the chemical treatment of cuticles to reach the end of products. However, the hardness, length, etc. differ depending on the race and individual differences, and it cannot be said that the material for factory products that must be guaranteed in quality is always perfect.

[0003]

SUMMARY OF THE INVENTION It is an object of the present invention to provide weaving with high heat resistance, which can be styled with a high temperature hair iron, using regenerated collagen fibers as a raw material for replacing human hair.

[0004]

That is, the present invention is a weaving made from regenerated collagen fibers, which comprises:
The present invention relates to weaving composed of regenerated collagen fibers having a shrinkage rate of 5% or less when using a curling iron at 60 ° C.

The regenerated collagen fiber is 40 to 140 ° C.
It is preferably obtained by heat-moisture treatment in.

The regenerated collagen fiber is preferably treated with a monofunctional epoxy compound and an aluminum salt.

The aluminum content of the regenerated collagen fiber is preferably 1 to 10% by weight.

[0008]

BEST MODE FOR CARRYING OUT THE INVENTION The constituent features of the present invention will be described below.

Usually, the temperature of the curling iron used when applying a hairstyle is about 160 to 200 ° C.
The weaving of the present invention has a shrinkage of 5% or less when using the above-mentioned hair iron at 160 ° C., so that the hairstyle can be applied as desired without causing melting or deformation of the hair tips. That is, it means that the shrinkage rate during the hair ironing treatment is 5% or less, and that the maximum hair ironing temperature at which the hair style can be applied is 160 ° C. or more, which does not cause melting or tip deformation.
It is particularly preferably 170 ° C. or higher. Shrinkage rate is 5%
If it exceeds, irregular waves are generated in the whole fiber and the hairstyle looks dirty. In particular, the shrinkage ratio at 160 ° C. is preferably 4.5% or less.

The curling iron temperature is measured as follows. (1) A fiber bundle (7.2 g / 45 cm) that has been well opened and adjusted to 160,000 dtex is folded in two and bundled with a thread, and the fiber bundle is cut off at a test length of 20 cm from the crevice to cut the fiber length. I got it. (2) Let it stand for 3 hours or more in a constant temperature and constant humidity environment (20 ° C., 65% RH). (3) Immediately before measurement, remove from the environment and measure as quickly as possible. (4) Fix the hair bundle to the head (head-shaped table),
A 0.8 g hair bundle is pulled out to make one measurement. (5) The root of the hair bundle is sandwiched with a flat iron heated to a predetermined temperature in the stove, and slowly slid toward the hair tip. (6) After that, curl the inner winding again from the root toward the tips of the hair so that it becomes a bob style. (7) After combing the tuft once with a comb, visually observe the state of melting and tip deformation to measure the length (Lcm) of the tuft. (8) The shrinkage rate S during the curling iron treatment is calculated by the following formula (I).
It was calculated according to. S = (20-L) x 100/20 (%) (I) (9) The maximum curling iron temperature with a shrinkage factor of 5% or less during hair ironing treatment and no melting or tip deformation is the curling iron temperature. did.

The general method for making weaving products is:
For example, a bundle of fibers of a specified length is sewn with a sewing machine for a wig to form a bundle of fibers processed into a waist-mino shape called weft or mino hair, which is wound on a pipe and desired for straight or spiral. Heat treatment to give the shape of the weaving product. Weaving products are used by knitting them in a net shape along the scalp and sewing them on their own hair, or by attaching them to the scalp and their own hair mainly in the form of strips with an adhesive or the like.

In the present invention, it is preferable to perform wet heat treatment at 40 to 140 ° C. in the process of processing regenerated collagen fibers to make weaving, unlike the above-mentioned ordinary heat treatment. By this moist heat treatment, the shrinkage of the fiber is as small as 5% or less even at a hair iron temperature of 160 ° C., and weaving without melting or hair tip deformation is obtained. Further, the water absorption rate is also reduced, and the regenerated collagen fiber when wet becomes stiff, and the wet feel is improved.

Here, the moist heat treatment means a heat treatment performed in the presence of water. The mist adjusted to a predetermined temperature may be sprayed by means such as a spray, or the regenerated collagen fiber may be left in a steam atmosphere adjusted to a predetermined temperature and immersed in water adjusted to a predetermined temperature. You may. For example, when treating at a temperature of more than 100 ° C., it is preferable to carry out in a steam atmosphere in an autoclave, and any known method can be used without limitation.

Specifically, the regenerated collagen fibers are fixed in advance in a desired shape (straight or spiral shape) and the temperature of the regenerated collagen fibers is adjusted to 40 to 140 ° C. in the presence of water. Treatment that can be held is preferable. The temperature of the fiber is measured by inserting a thermocouple inside the fiber bundle.

Although it is extremely difficult to determine the amount of water to be present on the surface of the regenerated collagen fiber when heat treating the regenerated collagen fiber in the presence of water, it is necessary to treat the regenerated collagen fiber uniformly. Therefore, it is preferable to adjust so that the water is present on the surface almost uniformly.

Further, the heat treatment in the presence of this moisture is 4
It is preferable to carry out at 0 to 140 ° C. Preferably, the lower limit is 50 ° C and the upper limit is 120 ° C. More preferably,
The lower limit is 70 ° C and the upper limit is 110 ° C. Most preferably, the lower limit is 80 ° C and the upper limit is 90 ° C. When the moist heat treatment temperature is lower than 40 ° C, shrinkage and deformation of the hair tips occur when the regenerated collagen fiber is styled with a hair iron at a temperature of 160 to 200 ° C, which tends to impair the commercial value. When the temperature exceeds 140 ° C, the regenerated collagen fibers tend to deteriorate.

The treatment time of the moist heat treatment needs to be appropriately adjusted depending on the atmosphere for treating the regenerated collagen fiber, the treatment temperature and the like. Usually 5 minutes or more, preferably 30
The wet heat treatment is preferably performed for at least 1 minute, more preferably for at least 1 hour. If the moist heat treatment time is shorter than 5 minutes, shrinkage and deformation of the hair tips occur when styling with a hair iron at a temperature of 160 ° C. or higher, and the commercial value tends to be impaired.

Next, the regenerated collagen fiber is dried. Drying is preferably 150 ° C or lower, more preferably 115
Carry out below ℃. If the drying temperature exceeds 150 ° C., the regenerated collagen fiber tends to deteriorate.

As a method of fixing the regenerated collagen fiber in a desired shape (straight or spiral shape) in advance, for example, a method of winding the regenerated collagen fiber around a pipe or a rod with a cloth tape or the like, 2
Examples thereof include a method of tensioning the regenerated collagen fiber between points or more fulcrums, and a method of sandwiching the regenerated collagen fiber between plates. The target shape is fixed,
Other methods may be used as long as water is sufficiently applied to the regenerated collagen fiber and the collagen fiber can be dried at a temperature of 60 ° C. or higher.

As a raw material for the regenerated collagen fiber used in the present invention, it is preferable to use the part of the floor skin. The floor skin is obtained from fresh floor skin obtained by slaughtering an animal such as cow or salted rawhide. Most of these floor skins and the like are composed of insoluble collagen fibers, but they are usually used after removing the fleshy portion adhered in a reticulated form and removing the salt used for preventing spoilage and deterioration.

Impurities such as glycerides, phospholipids, lipids such as free fatty acids, and proteins other than collagen such as albumin such as albumin are present in the insoluble collagen fibers. These impurities, spinning stability, quality such as gloss and strength and elongation,
It has a great influence on odor. Therefore, for example, the fat content in the insoluble collagen fiber is hydrolyzed by lime pickling, and the collagen fiber is unraveled, and then the conventional leather treatment such as acid / alkali treatment, enzyme treatment, and solvent treatment is performed. It is preferable that the impurities are removed in advance by removing the impurities.

The insoluble collagen treated as described above is solubilized in order to cleave the cross-linked peptide portion. As a method of such solubilization treatment, a generally adopted known alkali solubilization method, enzyme solubilization method, or the like can be applied.

When the alkali solubilization method is applied, it is preferable to neutralize with an acid such as hydrochloric acid.
As an improved method of the conventionally known alkali solubilization method, the method described in JP-B-46-15033 may be used.

The enzyme solubilization method has the advantage that regenerated collagen having a uniform molecular weight can be obtained, and is a method that can be preferably used in the present invention.
As such an enzyme solubilization method, for example, JP-B-43-2
The method described in Japanese Patent No. 5829 or Japanese Patent Publication No. 43-27513 can be used. Further, the alkali solubilization method and the enzyme solubilization method may be used in combination.

When the solubilized collagen is further subjected to operations such as pH adjustment, salting out, washing with water and solvent treatment, regenerated collagen having excellent quality can be obtained. It is preferable to perform these treatments.

The solubilized collagen obtained is, for example, 1
˜15% by weight, preferably 2 to 10% by weight, so as to obtain a stock solution having a solid content of about 10% by weight.
It is dissolved using an acidic solution adjusted to H2 to 4.5.
The obtained aqueous collagen solution may be subjected to defoaming under reduced pressure stirring if necessary, or may be filtered to remove fine dust which is a water-insoluble matter. The resulting solubilized collagen aqueous solution may further contain a stabilizer for the purpose of, for example, improving mechanical strength, improving water resistance and heat resistance, improving gloss, improving spinnability, preventing coloration, and preserving. An appropriate amount of additives such as a water-soluble polymer compound may be blended.

Regenerated collagen fibers are formed by discharging the solubilized collagen aqueous solution through, for example, a spinning nozzle or a slit and immersing it in an inorganic salt aqueous solution.
As the inorganic salt aqueous solution, for example, an aqueous solution of a water-soluble inorganic salt such as sodium sulfate, sodium chloride or ammonium sulfate is used, and the concentration of these inorganic salts is usually 10-4.
Adjusted to 0% by weight. The pH of the inorganic salt aqueous solution is usually 2 to 13, preferably 4 to 12 by adding a metal salt such as sodium borate or sodium acetate or hydrochloric acid, boric acid, acetic acid or sodium hydroxide.
It is preferable to adjust so that When the pH is less than 2 or exceeds 13, the peptide bond of collagen is likely to be hydrolyzed, and it tends to be difficult to obtain the target fiber. The temperature of the aqueous solution of the inorganic salt is not particularly limited, but it is usually desirable to be 35 ° C or lower. When the temperature is higher than 35 ° C, the soluble collagen is denatured and the strength of the spun fiber is reduced, which makes it difficult to manufacture a stable yarn. The lower limit of the temperature is not particularly limited, but usually can be appropriately adjusted according to the solubility of the inorganic salt. The fineness is also not particularly limited, but in consideration of being used for weaving, it is 30 to 100d.
tex is preferred. If the fineness is less than 30 dtex,
It tends to be too soft for hair. Again 100d
If it exceeds tex, it tends to be hard.

Further, in the present invention, it is preferable that the regenerated collagen fiber is made water resistant by reacting with an organic crosslinking agent or a metal salt. By such a treatment, coloring is reduced, and the water absorption rate is lowered, the moist feel is improved, the heat resistance is improved, and the moist heat treatment can be performed at a higher temperature. The temperature can be higher.

Of the above organic cross-linking agents, monofunctional epoxy compounds are preferable because they are less colored and have the effect of lowering the water absorption of the resulting fiber.

Specific examples of the monofunctional epoxy compound used here include ethylene oxide, propylene oxide, butylene oxide, isobutylene oxide, octene oxide, styrene oxide, methylstyrene styrene, epichlorohydrin, epibromohydrin. , Olefin oxides such as glycidol, glycidyl methyl ether, butyl glycidyl ether, octyl glycidyl ether, nonyl glycidyl ether, undecyl glycidyl ether, tridecyl glycidyl ether, pentadecyl glycidyl ether, 2-ethylhexyl glycidyl ether, allyl glycidyl ether, Phenyl glycidyl ether, cresyl glycidyl ether, t-butyl phenyl glycidyl ether, dibromophenyl glycidyl ether, benzyl group Examples of the present invention include glycidyl ethers such as sidyl ether and polyethylene oxide glycidyl ether, glycidyl formate, glycidyl acetate, glycidyl acrylate, glycidyl methacrylate, glycidyl benzoate and the like, and glycidyl amides. It is not limited to only. Among them, monofunctional epoxy compounds such as butylene oxide, octene oxide, styrene oxide, epichlorohydrin, butyl glycidyl ether, phenyl glycidyl ether, and glycidyl benzoate are highly reactive and can be treated in a shorter time. And is relatively easy to treat in water, so that it is preferably used.

The amount of monofunctional epoxy compound used is based on the amount of amino groups capable of reacting with the monofunctional epoxy compound in the regenerated collagen fiber measured by the amino acid analysis method.
0.1-500 equivalents, preferably 0.5-100 equivalents,
More preferably, it is 1 to 50 equivalents. When the amount of the monofunctional epoxy compound is less than 0.1 equivalent, the insolubilizing effect on the water of the regenerated collagen fiber is not sufficient. On the contrary, when the amount of the monofunctional epoxy compound exceeds 500 equivalents, the insolubilizing effect is satisfactory. However, it tends to be unfavorable in terms of industrial handleability and environment.

The monofunctional epoxy compound is used as it is or after being dissolved in various solvents. As the solvent, water; alcohols such as methyl alcohol, ethyl alcohol and isopropanol; ethers such as tetrahydrofuran and dioxane; halogenated organic solvents such as dichloromethane, chloroform and carbon tetrachloride; dimethylformamide (DMF), dimethylsulfoxide (DMSO) ) And other neutral organic solvents, and mixed solvents thereof may be used. When water is used as the solvent, an aqueous solution of an inorganic salt such as sodium sulfate, sodium chloride or ammonium sulfate may be used if necessary. Usually, the concentration of these inorganic salts is adjusted to 10 to 40% by weight. The pH of the aqueous solution may be adjusted, for example, by adding a metal salt such as sodium borate or sodium acetate, hydrochloric acid, boric acid, acetic acid, sodium hydroxide or the like. In this case, the pH is preferably 6 or higher, more preferably pH 8 or higher. When the pH is less than 6, the reaction between the epoxy group of the monofunctional epoxy compound and the amino group of collagen becomes slow and the insolubilization in water becomes insufficient. Also, such p
Since H tends to decrease with time, a buffer may be used if necessary.

The treatment temperature of the regenerated collagen fiber with the monofunctional epoxy compound is preferably 50 ° C. or lower. If the treatment temperature exceeds 50 ° C., the regenerated collagen fibers will be denatured and the strength of the obtained fibers will decrease, making it difficult to manufacture stable yarns.

Further, various additives such as a catalyst and a reaction aid may coexist. For example, examples of the catalyst include amines and imidazoles. Specifically, the amines include triethyldiamine, tetramethylguanidine, triethanolamine, N, N'-dimethylpiperazine, benzyldimethylamine, dimethylaminomethylphenol, 2,4,6-tris (dimethylaminomethyl) phenol. And secondary amines such as piperazine and morpholine; and quaternary ammonium salts such as tetramethylammonium salt, tetraethylammonium salt and benzyltriethylammonium salt. Examples of imidazoles include 2-methylimidazole, 2-ethylimidazole, 2-isopropylimidazole, 1-cyanoethyl-2-methylimidazole, 1-cyanoethyl-2-ethylimidazole, 1
-Cyanoethyl-2-isopropylimidazole, 2-
Ethyl-4-methylimidazole and the like can be mentioned. Examples of the reaction aid include salicylic acid or salicylic acid metal salt; thiocyanates such as thiocyanic acid and ammonium thiocyanate; tetramethylthiuram disulfide; thiourea.

Further, in the present invention, if necessary,
Wash the regenerated collagen fibers with water. Washing with water has the advantage that the inorganic salts contained during spinning can be removed.

Among the above-mentioned metal salts used for water resistance, aluminum salts are less colored, and the regenerated collagen fibers obtained have a firmness when wet.
The wet feel is improved, which is preferable. As a conventionally known method for improving the aluminum salt treatment, the method described in JP-A-6-173161 may be used.

The aluminum salt used here is not particularly limited, but examples thereof include aluminum sulfate, aluminum chloride, basic aluminum chloride, and basic aluminum sulfate. Here, basic aluminum chloride and basic aluminum sulfate are represented by the following chemical formulas (I) and (II).

[0038]

[Chemical 1]

(In the formula, N is 0.5 to 2.5) These aluminum salts can be used alone or in combination of two or more kinds. The aluminum salt concentration of this aluminum salt aqueous solution is aluminum oxide (Al ₂
It is preferably 1 to 10% by weight in terms of O ₃ ). If it is less than 1% by weight, the content of aluminum in the regenerated collagen fiber is small, the wet feeling becomes poor, and the shape imparting such as curl set becomes weak. On the other hand, if it exceeds 10% by weight, the treated fiber becomes hard and the texture is impaired.

The pH of the aqueous solution of aluminum salt is usually 2.5 to 6.5, preferably 2.5 to 6.5, using hydrochloric acid, sulfuric acid, acetic acid, sodium hydroxide, sodium carbonate or the like.
Adjust to 5.5. If this pH is less than 2.5, the structure of collagen tends to be destroyed and denatured.
If it exceeds, the aluminum salt will be precipitated, and it will be difficult for the aluminum salt to penetrate into the fiber. This pH can be adjusted, for example, by adding sodium hydroxide, sodium carbonate, etc., and is first adjusted to 2.2 to 5.0 to allow the aqueous solution of aluminum salt to penetrate into the regenerated collagen fiber, and then to 3 It is preferable to adjust to 0.5 to 6.5 to complete the treatment. When using a highly basic aluminum salt, the initial pH adjustment of 2.5 to 6.5 is sufficient. The liquid temperature of the aluminum salt aqueous solution is not particularly limited, but is preferably 50 ° C or lower. If the liquid temperature exceeds 50 ° C, the regenerated collagen fibers tend to be denatured.

The time for infiltrating the regenerated collagen fiber into the aluminum salt aqueous solution is 10 minutes or more, preferably 1-2.
5 hours. If the immersion time is less than 10 minutes, the reaction of the aluminum salt is difficult to proceed, and the wet feel of the regenerated collagen fiber is not sufficiently improved. Further, the upper limit of the immersion time is not particularly limited, but the reaction of the aluminum salt sufficiently progresses within 25 hours, and the wet feel becomes good.

In order to prevent the aluminum salt from being rapidly absorbed in the regenerated collagen fiber and causing unevenness in concentration, an inorganic salt such as sodium chloride, sodium sulfate or potassium chloride is appropriately added to the aqueous solution of the aluminum salt in an amount of 1 to 1.
You may add so that it may become a density | concentration of 20 weight%. Further, in order to improve the stability of the aluminum salt in water, an organic salt such as sodium formate or sodium citrate is appropriately added to the aqueous solution of the aluminum salt in an amount of 0.1 to 5% by weight, preferably 0.5 to 2% by weight. You may add so that it may become the density | concentration of%.

In the present invention, it is preferable to treat the fibers so that the aluminum content in the fibers after the treatment is 1 to 10% by weight. More preferable range is 3 to
It is 9% by weight. If the aluminum content is less than 1% by weight, the wet feel tends to be poor. On the other hand, if it exceeds 10% by weight, the treated fiber tends to be hard and the texture is impaired.

The regenerated collagen fiber thus treated with the aluminum salt is then washed with water, oiled and dried. Washing with water can be carried out, for example, by washing with running water for 10 minutes to 4 hours. As the oil agent used for oiling, for example, an oil agent composed of an emulsion of amino-modified silicone, epoxy-modified silicone, polyether-modified silicone or the like and a pluronic type polyether antistatic agent can be used. The drying temperature is preferably 100 ° C. or lower, more preferably 75 ° C. or lower, and the load during drying is 0.
01-0.25g weight, preferably 0.02-0.15g
It is preferably carried out under heavy gravity.

Here, washing with water prevents precipitation of the oil agent due to salt, or salt is precipitated from the regenerated collagen fiber during drying in a dryer, and the regenerated collagen fiber is broken or generated by the salt. This is to prevent the generated salt from scattering in the dryer and adhering to the heat exchanger in the dryer to lower the heat transfer coefficient. Further, when oiling is applied, it is effective in preventing the fibers from sticking and improving the surface property during drying.

[0046]

EXAMPLES Next, the present invention will be described in more detail based on examples, but the present invention is not limited to these examples.

The fineness, aluminum salt content and water absorption shown in the examples were evaluated by the following measuring methods.

(Fineness) Motorcycle Bro-type fineness measuring device De
nier Computer (registered trademark) DC-77A
The fineness was measured in an atmosphere having a temperature of 20 ± 2 ° C. and a relative humidity of 65 ± 2% by using (Search Corp.).

(Aluminum salt content) Regenerated collagen fiber was dried in a desiccator and then 0.1 g of this fiber was used.
Add 5 ml of nitric acid and 15 ml of hydrochloric acid to the solution and heat it.
Dissolved. After cooling, dilute this solution 50 times with water,
The aluminum content in the diluted aqueous solution was measured using an atomic absorption spectrometer (Z-5300 type) manufactured by Hitachi, Ltd.

(Water absorption rate) The water absorption rate was measured as follows. (1) The sample is left thin for 24 hours or more under the condition of room temperature of 20 ± 2 ° C. and humidity of 65 ± 2% RH. (2) Put 40 ml of the sample and deionized water in the sample bottle and cover. (3) Immerse in an incubator at 40 ° C. for 30 minutes (do not shake). (4) Use a pair of tweezers to quickly remove filter paper (Advantech Toyo Corp. qualitative filter paper No. 1, φ
(125 mm), insert the fiber, replace the filter paper, and remove the water adhering to the surface until the water does not soak into it. (5) Weigh the sample (W ₁ ). (6) A sample is put in a fully automatic dry heat sterilizer (Model MKM 2-2095 manufactured by Isuzu Seisakusho Co., Ltd.) adjusted to 105 ° C. and dried for 1 hour. (7) After allowing to cool in the desiccator for 30 minutes, the sample is weighed (W ₂ ). (8) The water absorption rate was calculated according to the following formula (II). Water absorption _{= (W 1 -W 2) /} W 2 × 100 (%) (II)

Example 1 A piece of calf skin was used as a raw material, and 30 parts was added to a piece of skin solubilized with alkali.
After adding an aqueous solution of hydrogen peroxide diluted to wt%, it was dissolved in an aqueous solution of lactic acid to prepare a stock solution having a pH of 3.5 and a solid content of 7.5% by weight. Stir defoamer under reduced pressure (Co., Ltd.)
Dalton, 8DMV type) was used for stirring and defoaming, transferred to a piston-type spinning stock solution tank, and allowed to stand still under reduced pressure for defoaming. After extruding such a stock solution with a piston, a fixed amount of gear pump solution was fed and filtered through a sintered filter with a pore size of 10 μm, then a pore size of 0.275 mm and a pore length of 0.5 m.
m through a spinning nozzle with 300 holes, sodium sulfate 2
Spinning speed 5 m / to a coagulation bath at 25 ° C. containing 0 wt% (adjusted to pH 11 with boric acid and sodium hydroxide)
Discharged in minutes.

Next, the obtained regenerated collagen fiber was
It was immersed for 4 hours at 25 ° C. in an aqueous solution containing 1.7% by weight of epichlorohydrin, 0.0246% by weight of sodium hydroxide, and 17% by weight of sodium sulfate (using neutral anhydrous sodium sulfate made by Tosoh Corporation). After that, the temperature of the reaction solution was further raised to 43 ° C. and the solution was immersed for 2 hours. After the reaction was completed, the reaction solution was removed, and then batch washing with water at 25 ° C. was performed three times. After this, aluminum sulfate (manufactured by Nippon Light Metal Co., Ltd.)
An aqueous solution containing 5.0% by weight of sulfuric acid band, 0.9% by weight of trisodium citrate (using purified sodium citrate M manufactured by Fuso Chemical Industry Co., Ltd.), and 1.2% by weight of sodium hydroxide. Dip at 30 ° C in 2 hours from the start of the reaction
After 3 hours and 4 hours, 5% by weight aqueous sodium hydroxide solution was added to the reaction solution. Then 25
Batch washing with water at 0 ° C was performed three times.

Next, a part of the produced fiber was immersed in a bath filled with an oil agent comprising an emulsion of amino-modified silicone and a pluronic type polyether antistatic agent to adhere the oil agent. It was dried under tension using a hot air convection dryer adjusted to 50 ° C. The obtained fiber was evenly spread on a newspaper in parallel with the axial direction of the pipe, wound on a pipe together with the newspaper, and fixed by winding a bandage on the pipe. Then, after subjecting it to an autoclave at 85 ° C (using a high pressure steam sterilizer HICLAVE HA-300P / V manufactured by Hirayama Seisakusho Co., Ltd.) for 1 hour, moist heat treatment was performed, and then a constant temperature blower thermostat adjusted to 115 ° C (Yamato Scientific Co., Ltd.) Made DN43)
And dried for 2 hours.

Example 2 In addition to the solid content concentration of the collagen stock solution being 7.0%,
An experiment was conducted in the same manner as in Example 1.

Example 3 In addition to the solid content concentration of the collagen stock solution being 8.0%,
An experiment was conducted in the same manner as in Example 1.

Example 4 An experiment was conducted in the same manner as in Example 1 except that the reaction time at 43 ° C. in the reaction of epichlorohydrin was 4 hours.

Example 5 An experiment was conducted in the same manner as in Example 1 except that the reaction time at 43 ° C. in the reaction of epichlorohydrin was 18 hours.

Example 6 Instead of treating with an aqueous solution containing epichlorohydrin, 1% by weight of formaldehyde adjusted to pH 9 with caustic soda,
30% at 25 ° C with an aqueous solution of 12.5 wt% sodium sulfate
An experiment was conducted in the same manner as in Example 1 except that the substrate was soaked for a minute.

Comparative Example 1 The same procedure as in Example 1 was carried out except that the moist heat treatment was not performed.

Comparative Example 2 The same method as in Example 2 was carried out except that the moist heat treatment was not performed.

Comparative Example 3 The same method as in Example 3 was carried out except that the moist heat treatment was not performed.

Comparative Example 4 The same procedure as in Example 4 was carried out except that the moist heat treatment was not performed.

Comparative Example 5 The same procedure as in Example 5 was carried out except that the moist heat treatment was not performed.

Comparative Example 6 The same method as in Example 1 was carried out except that the moist heat treatment was carried out at 30 ° C.

[0065]

[Table 1]

From the results shown in Table 1, it can be seen that by using the regenerated collagen fiber which has been heat-treated at 40 to 140 ° C., weaving that can be processed at a hair iron temperature of 160 ° C. or higher can be provided.

[0067]

By using the weaving using the regenerated collagen fiber of the present invention, compared to the human hair raw material market, which is extremely unstable in terms of quantitative security, quality, price, etc.,
High quality and uniform weaving can be supplied because raw materials of stable quality can be secured at all times.

Claims (4)

[Claims] 1. Weaving made from regenerated collagen fibers, which has a shrinkage of 5% or less when using a curling iron at 160 ° C. 2. The regenerated collagen fiber is 40 to 140.
The weaving according to claim 1, which is obtained by heat-moisture treatment at ° C. 3. The weaving according to claim 1 or 2, wherein the regenerated collagen fiber is treated with a monofunctional epoxy compound and an aluminum salt. 4. The weaving according to claim 3, wherein the regenerated collagen fiber has an aluminum content of 1 to 10% by weight.