JP2006182992A - Method for producing silk fine particle solution and silk fine particle powder and material containing silk fine particle - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a method for producing an odorless silk fine particle solution and silk fine particle powder from a silk fiber as a raw material and to obtain a material such as a food, a cosmetic and a fiber using the obtained silk fine particle. <P>SOLUTION: The odorless silk fine particle solution is obtained through a scouring process for subjecting a silk fiber to fixed scouring treatment and removing sericins attached to the silk fiber, a grinding process for mechanically grinding the obtained silk fiber into powder, a rubbing process for rubbing the obtained silk powder with roast salt and a process for predeterminedly desalting the obtained mixture. The silk fine particle powder is obtained by spray-drying or freeze-drying the silk fine particle solution. Since the solution and the fine particle powder are odorless, they are each favorably useful as an additive for a cosmetic, a food, etc., and a coating agent for a fiber. <P>COPYRIGHT: (C)2006,JPO&NCIPI

Description

  The present invention relates to a method for producing an odorless silk fine particle solution and silk fine particle powder using silk fiber as a raw material, and materials such as foods, cosmetics and fibers using the obtained silk fine particles.

  Silk yarn and accessory silk thread that are inappropriate for silk fabrics, etc., are formed from a protein-derived composition, and then powdered through a predetermined dialysis process such as hydrolysis and mechanical grinding. It is used as a coating agent for cosmetics, artificial leather, etc., and as a paste for cleaning finishing. However, in the conventional production method, the odor peculiar to amino acids is emitted when blended in an aqueous solution, a solvent, or the like due to protein modification or chemical reaction in the powder production process.

  In recent years, the habit of eating silk has been increasing due to health consciousness, and in order to extract highly accurate amino acids, production methods using enzymes such as chymotrypsin have been adopted. The silk powder cannot be expected to improve odor, and the demand for silk powder without odor is increasing.

  On the other hand, a method has been developed in which silk fiber is hydrolyzed with hydrochloric acid, subjected to deterioration treatment, and then mechanically pulverized to obtain silk powder (see Patent Document 1). However, since the silk powder produced by this method has a fibrous structure, it has a problem that it tends to have a non-uniform particle size and particle size, and when dispersed in a solution, it agglomerates and tends to be agglomerated.

JP-A-4-300309

  In view of the above circumstances, an object of the present invention is to provide silk fine particle powder with little odor, a solution thereof, and product materials such as cosmetics using the same.

  In the present invention, the method for producing a silk particle solution according to claim 1 includes a scouring step in which a predetermined scouring treatment is performed on the raw silk fiber to remove sericin adhering to the silk fiber, and the obtained silk fiber. Odorless silk through a pulverization step to mechanically pulverize the powder, a rubbing step of adding baked salt to the obtained silk powder and rubbing, and a step of subjecting the resulting mixture to a predetermined desalting treatment It is characterized by obtaining a fine particle solution. The silk fine particle powder production method according to claim 2 is characterized in that the silk fine particle solution obtained by the production method of claim 1 is subjected to spray drying treatment or freeze drying treatment to obtain silk fine particle powder. .

  The cosmetic according to claim 3 contains a silk fine particle solution obtained by the production method of claim 1 or a silk fine particle powder obtained by the production method of claim 2. Moreover, the foodstuff of Claim 4 contains the silk fine particle solution obtained by the manufacturing method of Claim 1, or the silk fine particle powder obtained by the manufacturing method of Claim 2. It is characterized by the above-mentioned. Furthermore, the fiber according to claim 5 is characterized in that the silk fine particle solution obtained by the production method of claim 1 or the silk fine particle powder obtained by the production method of claim 2 is coated on a fiber material.

  The silk fine particle solution and silk fine particle powder of the present invention can produce a silk fine particle solution and silk fine particle powder in a relatively simple process using silk waste fibers and the like as raw materials. Further, in the present invention, the odor peculiar to silk can be removed by adding baked salt to the silk material and rubbing it, so that a material suitable for use as a material for cosmetics, foods, fiber coatings and the like can be obtained.

  Hereinafter, preferred embodiments of the present invention will be specifically described. In the present invention, silk fibers such as silk waste fibers are used as a raw material. FIG. 1 shows a manufacturing process of the present invention. First, silk raw fiber as a raw material is roughly cut to shorten the fiber length. In this case, the fiber length after cutting is preferably about 0.2 to 0.8 mm. This is to facilitate powdering. If the fiber length after rough cutting is longer than this, it is difficult to obtain a preferable powder in the subsequent pulverization step, and conversely, it is inefficient to make it shorter than this.

  The roughly cut fiber is pulverized into powder using an appropriate pulverizer after removing sericin by a known scouring method. The fiber from which sericin has been removed becomes silk fibron fiber. As the pulverizer, for example, a ball mill can be used. The particle size after pulverization is preferably several microns, for example, about 8 microns.

  The silk powder obtained in the above pulverization process is blended with baked salt and, if necessary, a water-soluble slip binder as an additive for processing (preferably diethylene glycol) in an appropriate ratio and put into a kneader such as a convert mixer. Then, grind together with rubbing. The additive acts as a lubricant and a binder for imparting viscosity to silk powder and improving slipperiness. The baking salt is added to remove odor. Use of unbaked salt is deliquescent and cannot be rubbed together. Baked salt is suitable for rubbing silk particles because the particles are hard. The amount of these added is 4 to 8 kg of baked salt, preferably about 6 kg ± 0.5 kg, per 1 kg of silk powder. What is necessary is just to adjust suitably the compounding quantity of grilled salt according to a use, the property of a powder, etc. Depending on the case, it may carry out by about 6 to 10 times of silk powder. Moreover, diethylene glycol should just be about 15% by weight ratio with respect to the total amount of silk powder and baking salt.

  The blend of the silk powder, the baked salt, and the additive (diethylene glycol in the present embodiment) is rubbed using a suitable attritor. As this attritor, an attritor as illustrated in FIG. 2 can be preferably used. In this grinding machine, fixed blades 2 and rotating blades 3 are alternately arranged in a kneading and dispersing portion 1 a formed in a cylindrical casing 1, and the raw material powder supplied from a supply port 5 is fed by a feed screw 7. It is sent to the kneading and dispersing section, where it is kneaded by the rotation of the rotary blade. Examples of this type of device include those described in Patent Document 2, but other devices may be used as long as they can rub together silk powder.

JP 2002-1154 A

  By the kneading, the powder is rubbed in a sheared state to form a fine particle powder. The powder that has been rubbed is sent to the discharge port 9 and discharged from there. This step is repeated 2 to 4 times in order to obtain a fine particle powder having a particle size of about 2 microns. A slight odor remains at the stage where this rubbing process is repeated twice, but it becomes almost odorless if it is repeated four or more times. Moreover, the particle size of the silk powder can be further reduced by increasing the number of repetitions of the rubbing step. Depending on the conditions, it may be 1 micron or less.

  The mixture after the rubbing step is treated using a known desalting apparatus configured using an ultrafiltration membrane or an osmosis membrane in order to remove salt and diethylene glycol and impurities associated with silk powder. To obtain a high-quality silk fine particle aqueous solution. Since the obtained silk fine particle aqueous solution is odorless and has high purity, it can be used for various purposes as it is.

  Moreover, the silk fine particle aqueous solution obtained as described above can be dried using a spray-drying type drying apparatus or a vacuum drying apparatus to obtain silk fine particle powder. Since this powder is made of protein, it is necessary to control heat, temperature, etc. during drying.

  In the production process of the present invention, a large amount of purified water is added to the silk fine particle powder, and the water film covering the molecular membrane of the silk fine particle powder disappears through the process of desalting, dialysis, and filtration, and the water molecules By being attracted, it is presumed that sulfides such as methyl mercaptan and hydrogen sulfide, which cause odors, are dissociated and released into the aqueous solution and are not brominated.

  Silk fiber cut with a guillotine-type cutting machine to a fiber length of about 40 to 100 mm was used as a raw material. This raw material was immersed in an aqueous sodium carbonate solution (concentration 0.5%) heated to about 95 ° C. to remove sericin, and then washed with water and dried. This raw material consisting of silk fibron fibers from which sericin has been removed is further cut to about 0.2 to 0.8 mm with a rotary cutter, and then 80 hours with “Planet Ball Mill Machine” (trade name) manufactured by Seishin Enterprise Co., Ltd. Continuous processing. By this treatment, coarsely pulverized silk powder having a particle size of about 8 microns was obtained.

  12.5 Kg of baked salt is added to 1.25 Kg of the obtained silk powder, 1.375 Kg of diethylene glycol is added, and the mixture is put into a rotary blade type kneader (trade name convert mixer) and processed for about 4 minutes. Got.

  The obtained mixture was subjected to shearing grinding (rubbing) using a kneader Miracle KCK (trade name) manufactured by Asada Tekko Co., Ltd. The processing conditions were a spindle rotation speed of 40 rpm, 5 rotating blades, a blade clearance of 1.0 mm, a feed method being manually charged, a set temperature of 20 ° C., and a load value of 17 to 25 A.

  This grinding was repeated 4 times, and a dry mixture of 15.125 Kg and a particle size of 6.7 microns was recovered.

MOLSEP (trade name) manufactured by Daisen Membrane Systems Co., Ltd., type SUF is used as a desalination treatment device using purified water that has been purified with an apparatus equipped with a hollow fiber ultrafiltration membrane device. Desalting was performed using -108NS. The treatment condition was 9.6 m ³ / h three times. The ultrafiltration membrane was FN20-VP-FUC1582, the number of modules was 8, the power source was 5.5 KW, and the operating temperature was 40 ° C. or lower.

  By the above treatment, an odorless silk fine particle powder solution was obtained. Next, this solution was dried using FS-VS type vacuum dryer (trade name) manufactured by Fukae Pautech Co., Ltd. to obtain 1.15 kg of odorless silk fine particle powder.

  As a result of measuring the obtained odorless silk fine particle powder with a laser diffraction / scattering particle size measuring device LA-920 (trade name) manufactured by Horiba, Ltd., 48 to A particle size distribution containing 67% was obtained.

  The measurement conditions are the substance name silk powder, the sample preparation method is suspension, the circulation speed is 3, the dispersion medium ethanol, the particle diameter standard is volume, the 10% cumulative diameter is 0.4203 microns, the relative refractive index is 106a0001, the median diameter is 1.1876. The mode diameter was 0.5481 microns.

  The silk fine particle powder thus obtained was highly pure and odorless, so that it could be used satisfactorily as a food, cosmetic, fiber coating agent or the like.

  According to the present invention, since it is possible to remove the odor and cohesiveness of silk fine powder, which has been a problem in the past, the fields of use of conventional silk powder can be greatly expanded, and can be used in the cosmetics field, food field, etc. In addition, it is possible to easily obtain silk fine particle powder and solution that can be used as sanitary materials around the living body attached to the fiber composition.

It is a flowchart which illustrates the manufacturing process of this invention. It is sectional drawing which illustrates a kneading apparatus.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 Casing 2 Fixed blade 3 Rotating blade 5 Supply port 7 Feed screw 9 Discharge port

Claims (5)

  A scouring process in which the raw silk fiber is subjected to a predetermined scouring process to remove sericin adhering to the silk fiber, a pulverization process in which the obtained silk fiber is mechanically pulverized into a powder, and the resulting silk A method for producing a silk fine particle solution, characterized by obtaining an odorless silk fine particle solution through a rubbing step of adding baked salt to a powder and rubbing and a step of subjecting the resulting mixture to a predetermined desalting treatment.   A method for producing a fine silk particle powder, which comprises subjecting a fine silk particle solution obtained by the production method of claim 1 to a spray drying treatment or a freeze drying treatment to obtain a fine silk particle powder.   A cosmetic comprising the silk fine particle solution obtained by the production method of claim 1 or the silk fine particle powder obtained by the production method of claim 2. A food comprising the silk fine particle solution obtained by the production method of claim 1 or the silk fine particle powder obtained by the production method of claim 2.   A fiber comprising a silk fine particle solution obtained by the production method of claim 1 or a silk fine particle powder obtained by the production method of claim 2 coated on a fiber material.

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